I Have a Research Support System

On the new day, as usual, Xu Qiu made an appointment for morning exercise with his junior, and then took the school bus ahead of time to Zhangjiang.

Today is Friday, and the two of them didn't spend too long in the office, so they got ready and entered the laboratory.

After all, it is an organic synthesis experiment, and many of the experimental steps involved cannot be stopped once it starts, and must be done bravely.

For example, when crossing a pillar, it is impossible to stop halfway and wait a few days before continuing;

Another example is the post-reaction treatment. It is necessary to start the treatment, at least until the crude product comes out.

If you don't act swiftly, the night date between the two will be ruined——

This is their first official date.

Xu Qiu was in charge of the 24-hour halo reaction he voted for yesterday, and the reaction time is almost up now.

Such a very long response is generally not strictly accurate to minutes and seconds in actual operation, and even hour-level errors are allowed.

Time is mainly a reference, and the main basis is to see whether the reactants have reacted completely.

Xu Qiu walked to the fume hood, and did not rush to turn off the high-pressure mercury lamp for lighting. He dipped a small amount of solution in the reaction bottle with a capillary tube, and used the cross-point plate method to ignite a plate with the prepared raw material solution. .

A few minutes later, when Xu Qiu saw the result, he couldn't help shouting, "Damn it."

"Brother, what's the matter, did you fail the experiment again?" Han Jiaying said with concern, she put down her work as soon as she finished speaking, and hurried to Xu Qiu's side.

"No, on the contrary, the yield of this reaction is very high," Xu Qiu turned on the UV lamp when the school girl came over, pointed to the silica gel plate, and said, "Look at the sample points representing the raw materials in the product, which are as shallow as almost I can’t see it anymore, and the product spot, several other by-products, all disappeared overnight, leaving only one main product with a very dark color.”

"Hmm..." Han Jiaying nodded, "Indeed, the production rate is estimated to be around 90%."

"Almost," Xu Qiu smiled, "Maybe it's because I failed a reaction yesterday and accumulated a wave of character, so I'm going to change my luck today."

"Then I'll go get busy." Seeing that there was nothing wrong with him, Han Jiaying didn't stay any longer.

Her task today is also very arduous. She synthesized a new batch of PDI monobromine substitution products before, and some of them are still in the sample mixing stage. Today, she has to separate and purify them all, which can be regarded as an assistance to Xu Qiu;

She also needs to complete the category she is responsible for in the second part of the review, and hand it over to Xu Qiu for integration.

"Go." Xu Qiu raised his hand and waved it. Originally, he wanted to pat the junior girl to kill him, but he stopped in time when he remembered that he was still wearing several layers of gloves and didn't know what medicine had been stained on it. The car, there are many restrictions in the laboratory, it is not a good place to talk about love.

After the junior girl left, he stared at the silicone plate on the lab table, lost in thought.

The photocyclization reaction in front of us has no other reaction sites except the fused ring at the central core unit, and the main product must be the fused ring structure we need.

There are no by-products in the product, and the difficulty of separation and purification is not high.

Moreover, the yield is also high, and the final product yield may be more than 50 mg.

If nothing else, it can be regarded as a great success of the experiment.

if it is like this……

You can change the experimental path.

Bring 15 mg back to Handan for experimentation as last time, and keep the rest of the product for further optimization.

As long as there is more than 15 mg of the final product of the next reaction, it is sufficient.

Well, the plan works.

After planning the experimental route, Xu Qiu turned off the high-pressure mercury lamp and started the post-reaction treatment.

Because the room is also illuminated by fluorescent lamps, which can also provide energy for the photocyclization reaction, even if the high-pressure mercury lamp is turned off, the reaction is still in progress.

To completely shut down the reaction, the iodine elemental catalyst in the reaction flask must be removed.

More than that, simple iodine is soluble in toluene solvent, if it is not removed, it will be mixed in the product, which may affect the subsequent separation and purification steps.

Before the crude product is put on the silica gel column, it is better to ensure that there are not too many strange things in it.

As for the method of removing iodine, Xu Qiu checked the information in advance and kept it in mind.

He first prepared a saturated aqueous solution of sodium sulfite, then added it to the reaction flask and shook it slightly.

Elemental iodine, sodium sulfite, and water react, and the resulting products, sodium sulfate and hydrogen iodide, dissolve in water.

Next, separate the organic phase (toluene) and the aqueous phase with a separatory funnel, wash with saturated aqueous sodium sulfite three times to ensure that there is no iodine residue, and then separate to obtain a toluene solution of the product.

According to the product estimation of 50 milligrams again, add the silica gel powder of corresponding quality and mix.

Finally, the solvent was rotovapped.

The solvent used for spin evaporation this time is toluene, which has a boiling point of about 110 degrees Celsius, which is higher than water, so it is not so easy to spin dry.

If not handled properly, the end product will be a sticky, oily liquid.

Decompression is a must, as is warming up.

Xu Qiu raised the temperature of the water bath next to the rotary evaporator to 80 degrees Celsius, heated the rotating eggplant-shaped bottle, and cooperated with the water pump to depressurize and pump continuously for more than an hour.

Finally, a dry, sample-mixed product was obtained.

On the way, Chen Wanqing arrived at the laboratory. For some reason, she arrived half an hour later than usual.

She greeted Xu Qiu and the others, chatted for a while, and started her own experimental work.

...

In the afternoon, Xu Qiu completed the separation and purification of PDI3-B-5X photocyclization reaction products with liquid chromatography.

Because there were not many samples, it didn't take too much time. In the end, about 55 mg of the product was obtained, which was still a red powdery solid, and the yield was 88%.

The new product obtained is named PDI3-BX-5, where PDI3 represents 3 PDI molecules, B represents the benzene ring, X represents the connection of fused rings, and 5 represents the side chain on the nitrogen atom of the PDI molecule is a symmetrical dendritic structure, Each branch is an alkyl group of 5 carbon atoms.

Xu Qiu copied the new material into the simulation laboratory, and immediately arranged for model demonstrators to start exploring the performance of the device.

Then go back to the office and start the paper work, the task is to put together the content of the second part of the review.

He had already got the part that Han Jiaying was in charge of at noon. The junior girl didn't lie to him yesterday, saying that she was almost finished, but it was really just a little bit, not a billion bit.

After a general look, the part of the school girl is much easier to change than the school girl.

Even so, it is a time-consuming and labor-intensive task.

It wasn't until after five o'clock in the afternoon that the work was barely completed.

"It's finally done." Xu Qiu pressed Ctrl+S to save the file, and then pressed WIN+L to lock the computer screen, took a long breath, and shook his head.

After staring at the screen for a long time, his consciousness is a little blurred. Compared with writing articles, he still prefers to do experiments.

Looking around, he was the only one in the office at this time.

I vaguely remember that Chen Wanqing finished the experiment at about 4:40, because it was Friday and he took the school bus back to Handan ahead of schedule.

I don't remember what Han Jiaying said, she should still be working in the laboratory.

Xu Qiu lifted his trousers and felt his bladder explode, so he went to the bathroom in the corridor.

The Zhangjiang Microelectronics Building was built only in recent years, so the bathroom decoration is very luxurious, and it is cleaned regularly every day. The area is dozens of square meters, and the tiles are shining brightly.

There are six pits in the men's toilet, and the women's toilet... I don't know, I haven't been there.

However, there is only Teacher Wei's research group on the entire floor, and Xu Qiu and the others are the only ones doing activities. There are three or two big cats and kittens, which is really a bit wasteful.

After solving the physical problems, Xu Qiu walked back to the A502 laboratory.

When he walked to the door of the laboratory, he suddenly had an idea, slowed down his pace, quietly put on a clean lab coat, and then glanced at Han Jiaying's position.

She was sitting next to the liquid chromatography instrument, staring at the computer screen, her body curled up slightly, and she seemed a little tired.

The direction the two are facing just presents a 90-degree angle. Although their backs are not exactly facing each other, there is still room for manipulation.

Xu Qiu tiptoed towards the target, and the vibrating sound of the surrounding equipment covered up the sound of his footsteps.

Soon he came behind the school girl.

Target doesn't seem alert, good chance!

"Eat me with a righteous backstab!" Xu Qiu put his arms around the junior girl, and then rested his head on her hair.

"Ah, I was hit." Han Jiaying smiled and cooperated deliberately.

"When did you find out..." Xu Qiu looked up and saw his image on the glass, "So that's how it is."

Han Jiaying moved her head and motioned Xu Qiu to look at the computer screen, "Brother, today will be a little later. This sample has just started, but it is the last sample. More than 2 grams have been prepared."

"Nice job," Xu Qiu said happily, and couldn't help but hug the school girl in his arms even tighter.

"Ah... Brother, please be gentle, I can hardly breathe..."

"What kind of words are these tigers and wolves?" Xu Qiu hurriedly reduced the strength of his hand, thinking to himself, "In this way, for a long time, there will be no need to worry about the shortage of basic raw materials."

‘For the three main PDI raw materials, to achieve the step of bromine substitution, and then obtain the pure monobromine substitution, it needs to pass through the column six times, and they are all products in large quantities, so the experimental pressure is not small. '

'I've been busy with my own affairs for the past few days, basically I didn't help her, and I didn't ask too much about the progress of her experiment. I only know that she is progressing smoothly. I didn't expect to give me such a surprise now. '

'By the way, I want to ask about tonight's date. I originally planned to go back to Handan directly after the experiment, but now the plan has changed...'

"When we go back to Handan, should we find a place in Zhang Jiang?"

"Hmm..." Han Jiaying thought for a while and said, "Let's go back to Handan, where we are more familiar."

Next, the two cooperated and cooperated tacitly, and it took more than an hour to complete the experiment.