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

HRID 1780211ノート

反応式

HRID 1780211 の反応式
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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-5b09261e40aa4a84aeb5d54b71602beb
出典データセット
uspto-grants-1997_05
特許番号
US05629432

反応ノート

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