Ethanol → Ethyl 3-cyano-3-phenylpropanoate

HRID 1076882노트

반응식

HRID 1076882 반응식
C(OC(=O)[C:5](=[CH:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:6]([O:8][CH2:9][CH3:10])=[O:7])C.[C-:19]#[N:20].[K+].C(O)C>O>[CH2:9]([O:8][C:6](=[O:7])[CH2:5][CH:11]([C:19]#[N:20])[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1)[CH3:10]

참가 물질

5

반응물 3

HCID 702EthanolHCID 9032Potassium CyanideHCID 94751Diethyl (phenylmethylene)malonate

생성물 1

HCID 12414061Ethyl 3-cyano-3-phenylpropanoate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

120 g of benzalmalonic acid diethyl ester, 33.6 g of potassium cyanide, 1600 cc of ethanol and 160 cc of water are stirred at a bath temperature of 60° for 12 to 14 hours. The reaction mixture is then cooled with ice water, the potassium bicarbonate which crystallizes is filtered off, the filtrate is made neutral with about 15 cc of 1 N hydrochloric acid, air is passed through the solution with a water jet vacuum pump for 1 hour, the solvent is distilled off on a rotary evaporator, 100 cc of water are added to the oily residue, and extraction is effected 6 times with 250 cc amounts of ether. The 3-cyano-3-phenyl-propionic acid ethyl ester, obtained after distilling off the ether, is purified by vacuum distillation. B.P. 125°-130°/0.15 mm Hg.

후처리

  1. customthe potassium bicarbonate which crystallizes
  2. filtrationis filtered off
  3. distillationthe solvent is distilled off on a rotary evaporator, 100 cc of water
  4. additionare added to the oily residue, and extraction

출처 및 근거

ORD 기록
ord-d6029a477334409b996241ed14078935
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03958003

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