I Have a Research Support System
Chapter 440
Xu Qiu and Han Jiaying held hands and walked into the organic laboratory on the fifth floor.
After a few months, Xu Qiu smelled the familiar smell of solvent again, and Xu Qiu really missed it. He skillfully put on protective equipment such as lab coat, three-layer protective gloves, and disposable activated carbon mask.
These basic experimental skills have long since become muscle memory.
Xu Qiu didn't wear the gas mask anymore, it was too troublesome to wear, and the experiment to be carried out today was not very dangerous.
The synthesis steps of PTQ1 are relatively simple, only three steps are required:
In the first step, "3,6-dibromo-4,5-difluorobenzene-1,2-diamine", referred to as "hexa-substituted benzene", is reacted with glyoxylic acid and acetic acid at room temperature, and the benzene ring The two amino groups above are cyclized to a six-membered ring heterocycle, namely 1,4-azabenzene, thereby obtaining a condensed ring structure formed by benzene and 1,4-azabenzene.
In the second step, the product obtained in the first step is reacted with 1-bromo-2-hexyldecane under the action of potassium tert-butoxide, the purpose of which is to introduce an alkoxy side chain to obtain a mono body unit. This unit is an A unit that tends to withdraw electrons, and was named Q by Xu Qiu, mainly because the shape of its molecular structure is very similar to the letter Q.
In the third step, the Q unit substituted by dibromo and the thiophene unit T substituted by trimethyltin were subjected to Stille coupling reaction to obtain the conjugated polymer donor material PTQ1.
PTQ series donors, because the structure is relatively simple, the only place that can be regulated is the alkoxy side chain connected to 1,4-azabenzene, and a vacant reaction site next to the side chain.
For example, the vacant reaction sites on PTQ1 materials are hydrogen atoms, which can be replaced by various other groups, such as methyl groups, fluorine atoms, chlorine atoms, and another side chain. This is what the school girl will be responsible for in the future.
Xu Qiu and Han Jiaying each occupied an adjacent fume hood, and planned to vote the same response independently.
In fact, Han Jiaying's experimental skills in the synthesis of body materials are no longer weaker than Xu Qiu's. Both of them have reached the fifth level of proficiency, and the gap is not that big.
Rather than saying that Xu Qiu is guiding Han Jiaying, it is safer to say that the two of them synthesized together. As long as there is no problem with the raw materials, the chance of experiment failure is too low.
As for why Xu Qiu didn't hand over the job directly to the school girl, it was because he also wanted to warm up and then synthesize the Y series receptors.
If he was away from the frontline for a long time to do experiments, the probability of success in the synthesis reaction would be reduced. He didn't want to waste too much time because of the failure of the experiment when synthesizing the Y series receptors.
Start experimenting.
Xu Qiu first took a clean two-necked flask, and then added 906 mg of hexa-substituted benzene, 222 mg of glyoxylic acid, and 30 ml of acetic acid into it, and then heated the mixture to 40 degrees Celsius. After 10 minutes, the The solution was brought to room temperature and stirring was continued for 3 hours.
This step of the experiment is relatively simple, and there is no need to distill the solvent, and the raw materials purchased can be used directly.
Among them, a new material - glyoxylic acid is involved.
Glyoxylic acid is a white crystal with a melting point of about 98 degrees Celsius. It is an intermediate of medicine, dyes, plastics and pesticides. It has low toxicity. According to the MSDS manual, it emits an unpleasant smell.
However, when Xu Qiu weighed the glyoxylic acid, he operated it behind a fume hood, so he didn't smell any special smell.
In contrast, the taste of acetic acid is more pungent and full of vinegar.
It is also easy to understand, after all, acetic acid is a liquid, and it is easier to volatilize.
At noon, the three of them went to Jiangwan canteen for lunch.
Now the second floor of the cafeteria on the Jiangwan side is open. The quality of the dishes has indeed improved slightly, and the variety of choices has also increased. New additions include fried rice, fried noodles, fried rice noodles, spicy hot pot, and braised chicken and rice. , braised short ribs and other dishes.
In the afternoon, after the reaction was completed, Xu Qiu filtered and collected the precipitate obtained from the reaction with a Buchner funnel, and dried them in a vacuum oven to obtain a large amount of white solid.
Xu Qiu weighed the crude product, and it was 1.1 grams. The yield of this reaction is really not low.
Considering that the side reaction products of this step reaction and the remaining small amount of raw materials will not affect the next second step reaction, Xu Qiu directly weighed 1 gram of the white solid just obtained, and mixed it with 395 mg of tert-butyl Potassium alkoxide was mixed with 897 mg of 1-bromo-2-hexyldecane and dissolved in 30 ml of methanol solvent.
The role of 1-bromo-2-hexyldecane is to introduce side chains.
Potassium tert-butoxide is an important organic base used to provide an alkaline reaction environment. Its alkalinity is stronger than that of potassium hydroxide, and the alkalinity of potassium hydroxide is stronger than that of sodium hydroxide. Hydroxide Sodium is very common and is caustic soda.
Here, Xu Qiu once again thought of the chicken feet that were poisoned by sodium hydroxide solution in middle school.
This step of reaction is not difficult. It only needs to be heated and refluxed at 90 degrees Celsius for 12 hours. There is definitely no way to deal with the reaction today, so we can only wait until tomorrow morning.
In his free time, Xu Qiu plans to purchase raw materials for the synthesis of Y-series receptors, including dibromo-substituted NT units and mono-trimethyltin-substituted TT units.
The first thing he thought of was the Blue River Optoelectronic Material Company in which he was a shareholder, so he contacted Yang Qin, but the other party told Xu Qiu in embarrassment that what he wanted was out of stock.
However, Yang Qin brought good news: "Ma Weiwei's research group at Anseong Jiaotong University purchased one gram of IEICO-4F and one gram of ITIC-4F, and two other research groups also purchased some materials. It is a 'poor group' who only buys one or two hundred milligrams at a time, but it can be regarded as a good start."
"In addition, the company recently recruited a new master student and an undergraduate student, and the team has also begun to grow larger."
No matter what, the materials still have to be bought. My company is out of stock, so I can only find the Shencheng Optoelectronics company I cooperated with before.
Xu Qiu asked straight to the point: "I want to buy the NT unit substituted by dibromine and the TT unit substituted by monotrimethyltin. The product numbers are NT7 and TT10 respectively. I will buy 500 mg of each."
The salesman replied quickly: "NT7 is 2200 per gram, TT10 is 1200 per gram, and the price of 500 mg is 1200 and 700 respectively. If there is no problem, the warehouse will transfer the goods here."
Xu Qiu: "No problem."
Sales: "Dear, why don't you come here to get the goods recently? We have newly released IEICO-4F and IDIC, and the efficiency can reach more than 12%. Do you want to know more? If you don't need finished products, we also have monomers. It can be sold."
Sales: "[Hottest Products in November.jpg]"
Xu Qiu: "..."
Xu Qiu: "Do you have a common QQ account at work?"
Sales: "Yes."
Xu Qiu: "These two materials were developed by our group."
Sales: "Ah, sorry to bother you."
Sales: "The goods here have been packed for you, and they will be sent out by express delivery today. Please have a happy life and smooth scientific research."
Xu Qiu: "OK"
It is true that Xu Qiu from Shencheng Optoelectronics Company has not visited for a long time, and now the article does not include the name of the other party, but the name of Blue River Optoelectronics Material Company to promote his company.
Blue River heard that Shencheng Optoelectronics Company had a reward for publishing articles, and immediately said that we do the same here, and the reward amount is 1.5 times theirs, and told Yang Qin the reward rules to let him promote it.
Therefore, the prize money for each article of organic photovoltaic in the group has not decreased but increased.
In the evening, Xu Qiu took Han Jiaying and Wu Shengnan to eat a bowl of Jiangwan's braised beef noodles, and gave the two of them this treasure shop, and finally got unanimous praise from the two girls.
Although the Jiangwan canteen has been renovated and re-contracted, the quality of the dishes is not bad, but compared to before, if compared with the Handan campus, it is not even as good as the canteen in the south area, let alone the canteens in the headquarters and the north area. .
It can be said that "Jiangwan people have suffered from the canteen for a long time." Xu Qiu estimated that when the graduate students of science and engineering moved in, the canteen here would most likely be rectified again.
On Tuesday morning, Xu Qiu came to the Jiangwan laboratory to handle the reaction. He poured the reaction mixture into a saturated ammonium chloride solution, extracted it with dichloromethane, and washed it with water, three times.
The obtained organic extract was dried by adding anhydrous magnesium sulfate, then filtered, and the solvent was evaporated to dryness by rotary evaporation to obtain a reaction crude product.
In most of the previous cases, the reaction product was solid powder, but this time the crude product was unique, a colorless oily product.
Originally, Xu Qiu thought that he hadn't done synthesis after a few months, and his strength had declined, which led to the failure of the experiment.
Later, seeing that the product that the school girl got was the same as him, I felt relieved.
Two people get the same result, there is a high probability that there is no problem.
It's like two academic masters who got the answers right after the exam and found that the answers to all the questions are the same, then it's probably stable, and both of them got perfect marks.
And if two scumbags get the answers right after the exam and find that all the answers to the questions are the same, it will be a little scary...
Next, the crude product is passed through a column for further purification to obtain the final product.
The yield of this reaction was very high, Xu Qiu's yield was 91%, and Han Jiaying's was 90%.
The difficulty in the synthesis of PTQ1 is mainly on the Q unit, and the subsequent reaction between the Q unit and the T unit is a simple Stille coupling reaction.
Therefore, Xu Qiu did not intend to participate in the next synthesis, and his hands were hot now, so he began to focus on writing the "Joule" article.
However, on Wednesday, Xu Qiu still ran to the Jiangwan campus, pretending that he was doing experiments, and he had tasted the sweetness.
Teacher Wei is usually in the Handan campus. He often goes to the 216 laboratory to inspect and arrest people. He only calls to inquire about very important matters.
Now it's really cool to stay away from Wei Xingsi and stay in the bend of the river, and generally you won't be caught.
On Thursday morning, when Xu Qiu was in class, he suddenly received a call from Wei Xingsi. After he hung up, he was about to send a text message. Wei Xingsi called again. After hanging up again, Wei Xingsi took the initiative to send a text message:
"Joule and AM's article comments came at the same time, and I will forward the email to you immediately."
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