Reaction scheme:
Synthesis:
1. 2-bromo-4-methylpropiophenone 2 kg and 4 liters of ethyl acetate was stirring in the reactor.
2. Added 1900 g pyrrolidine into the drop funnel and mounted on the reactor cover.
3. Open tap drop funnel and added pyrrolidine dropwise, with intense stirring.
4. Check temperature below 65 *C.
5. After all pyrrolidine added, inteximally stirred 1 hour.
8. Turn on reactor vacuum pump, and chiller pump for reactor condenser.
9. Distilled all or most amount of ethyl acetate.
10. Stop vacuum pump and added in the reactor acetone. Stirring continues.
11. Added hydrochloric acid into the drop funnel and mounted on the reactor cover.
12. Dropwise acid to pH - 5. Drain a small amount from the bottom reactor tap and control the level of acidity with a litmus strip. Returns the sample to the reaction mixture.
13. After that, poured all mixture in bucket and put in the freezer for 12 hours.
14. Installed by vacuum filtration system (nutsche filter, filter cloth, vacuum pump).
15. Start vacuum pump.
16. Pour a bucket from step 13 to the filter bowl.
17. Filter and press until the mixture of the bowl becomes solid.
18. Pour cold acetone into the bowl to cover the whole solid from above.
19. Filter all acetone. Repeat step 18 if the solid is not white.
20. After filtered all acetone and achieving white solid, put the contents of the bowl in the glass containers for drying.
21. Put the glass containers on racks at room temperature.
22. Dry to constant mass. Periodically mix and grind, for faster drying.
Synthesis:
1. 2-bromo-4-methylpropiophenone 2 kg and 4 liters of ethyl acetate was stirring in the reactor.
2. Added 1900 g pyrrolidine into the drop funnel and mounted on the reactor cover.
3. Open tap drop funnel and added pyrrolidine dropwise, with intense stirring.
4. Check temperature below 65 *C.
5. After all pyrrolidine added, inteximally stirred 1 hour.
8. Turn on reactor vacuum pump, and chiller pump for reactor condenser.
9. Distilled all or most amount of ethyl acetate.
10. Stop vacuum pump and added in the reactor acetone. Stirring continues.
11. Added hydrochloric acid into the drop funnel and mounted on the reactor cover.
12. Dropwise acid to pH - 5. Drain a small amount from the bottom reactor tap and control the level of acidity with a litmus strip. Returns the sample to the reaction mixture.
13. After that, poured all mixture in bucket and put in the freezer for 12 hours.
14. Installed by vacuum filtration system (nutsche filter, filter cloth, vacuum pump).
15. Start vacuum pump.
16. Pour a bucket from step 13 to the filter bowl.
17. Filter and press until the mixture of the bowl becomes solid.
18. Pour cold acetone into the bowl to cover the whole solid from above.
19. Filter all acetone. Repeat step 18 if the solid is not white.
20. After filtered all acetone and achieving white solid, put the contents of the bowl in the glass containers for drying.
21. Put the glass containers on racks at room temperature.
22. Dry to constant mass. Periodically mix and grind, for faster drying.
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