The chemical industry reduces the impact on the environment during synthesis 126764-17-8. I believe this compound will play a more active role in future production and life.
The chemical industry reduces the impact on the environment during synthesis 126764-17-8, name is 1-Chloro-6,6-dimethylhept-2-en-4-yne, I believe this compound will play a more active role in future production and life. 126764-17-8
29 kg of N-methyl-1 -naphthalene methylamine hydrochloride was charged into a reactor containing 70.4 liters of dimethylformamide and 11 liters of water, under stirring. The contents were stirred for 15 minutes for clear dissolution and 11 kg of sodium carbonate was added to it. The reaction mass was cooled to 13 EPO C and 22 kg of 1-chloro-6,6-dimethyl-2-heptene-4-yne was added slowly at 11 to 14 C. The reaction mixture was stirred at 12 to 14 0C for 60 minutes and then heated to 55 0C. The reaction mass was maintained at 60 C for 5 hours and reaction completion was confirmed by thin layer chromatography. The reaction mass was cooled to room temperature and 99 liters of water was added. Reaction mass was extracted three times with a total of 75 liters of dichloromethane (3×25 liters). Total organic layer was washed twice with 88 liters of water (2×44 liters); 18 liters of water was charged to the final organic layer and was cooled to 13 0C. Reaction mass pH was adjusted to 0.2 by adding 15 liters of 36% aqueous hydrochloric acid and stirring for 30 minutes. The organic layer was separated and washed three times with a total of 267 liters of water (3chi89 liters). Final organic layer was transferred into a reactor and the solvent was distilled completely below 45 C. 11.8 liters of petroleum ether was charged and the solvent distilled completely at below 50 C. Again 68 liters of petroleum ether was charged and heated to reflux. The mass was stirred at reflux for 30 minutes and cooled to 50 C. The solid thus formed was allowed to settle for 60 minutes and the top petroleum ether layer was decanted. The decantation process was repeated two more times. Finally 44 liters of petroleum ether was charged, heated to reflux, maintained for 30 minutes at reflux and then cooled to 25 C. The contents were stirred for 60 minutes at 20 to 25 0C and centrifuged to recover the solid. The centrifuged solid was washed twice with petroleum ether (2×16 liters) and spin- dried for about 60 minutes to get 29.3 kg of crude terbinafine hydrochloride as a semi-dry solid.
The chemical industry reduces the impact on the environment during synthesis 126764-17-8. I believe this compound will play a more active role in future production and life.
Reference:
Patent; DR. REDDY’S LABORATORIES LTD.; DR. REDDY’S LABORATORIES, INC.; WO2007/44273; (2007); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics