1-Acetoxy-2-bromoethane → Diethyl alpha-phenyl-alpha-(2-acetoxyethyl)malonate

HRID 1780211노트

반응식

HRID 1780211 반응식
CC(C)([O-])C.[K+].[C:7]1([CH:13]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[C:24]([O:27][CH2:28][CH2:29]Br)(=[O:26])[CH3:25]>CN(C=O)C.O>[C:7]1([C:13]([CH2:29][CH2:28][O:27][C:24](=[O:26])[CH3:25])([C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1

참가 물질

6

반응물 3

HCID 135641-Acetoxy-2-bromoethaneHCID 66514Diethyl phenylmalonateHCID 23665647Potassium tert-butoxide

생성물 1

HCID 19050130Diethyl alpha-phenyl-alpha-(2-acetoxyethyl)malonate수율 100.8%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

A solution of potassium tert.butoxide (448 g, 4M) in DMF (2 l) under nitrogen at room temperature was treated dropwise with diethyl phenylmalonate (945 g, 4M). 1-Acetoxy-2-bromoethane (668 g, 4M) was added. The reaction was allowed to cool to room temperature after 45 mins and was diluted with water (5 l) then extracted with IPE (2 l, 500 ml). The extracts were washed, dried and evaporated to give the title compound (1300 g). Bp 130°/0.05 mm.

후처리

  1. extractionthen extracted with IPE (2 l, 500 ml)
  2. washThe extracts were washed
  3. customdried
  4. customevaporated

출처 및 근거

ORD 기록
ord-5b09261e40aa4a84aeb5d54b71602beb
출처 데이터셋
uspto-grants-1997_05
특허 번호
US05629432

반응 노트

불러오는 중…