반응 #213864
ord-92d69f50b91f450fb5744ced5dbdbe85
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후처리
- 1온도was warmed to 40°
- 2온도maintaining a reaction temperature of about 40°
- 3세척after which it was washed with an aqueous solution
- 4workup.ADDITIONcontaining 20% sodium carbonate
- 5기타The organic phase was separated from the mixture
- 6기타the solvent removed by distillation under reduced pressure
실험 절차
A stirred mixture of sodium cyanide (18.0 g, 0.36 mole) and 3-(cyclohexylamino)propanesulfonic acid (1.34 g, 0.006 mole) in 300 ml of water was warmed to 40°. During a one hour period, maintaining a reaction temperature of about 40°, a solution of cis-3-(2,2-dichloroethenyl)-2,2-dimethylcyclopropanecarbonyl chloride (71.7 g, 0.315 mole) and 3-phenoxybenzaldehyde (61.9 g, 0.3 mole) in 262.2 g of n-heptane was added. The mixture was then stirred at 40° for one additional hour, after which it was washed with an aqueous solution containing 20% sodium carbonate and then with water. The organic phase was separated from the mixture and the solvent removed by distillation under reduced pressure to give α-cyano-3-phenoxybenzyl cis-3-(2,2-dichloroethenyl)-2,2-dimethylcyclopropanecarboxylate.