Diethyl [(2-bromophenyl)methylidene]propanedioate → Ethyl 3-(2-bromophenyl)-2-ethoxycarbonyl-3-methylpropionate

HRID 1585968

反応式

HRID 1585968 の反応式
[CH2:1]([O:3][C:4]([C:6](=[CH:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[Br:19])[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5])[CH3:2].[CH3:20][Mg]Br>CCOCC.[Cl-].[NH4+].[Cu](Br)Br>[Br:19][C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=1[CH:12]([CH3:20])[CH:6]([C:7]([O:9][CH2:10][CH3:11])=[O:8])[C:4]([O:3][CH2:1][CH3:2])=[O:5]

参加物

6

反応物 2

HCID 246693Diethyl [(2-bromophenyl)methylidene]propanedioateHCID 178418573HCID 178418573、化合物

生成物 1

HCID 21217382Ethyl 3-(2-bromophenyl)-2-ethoxycarbonyl-3-methylpropionate

試薬・触媒・溶媒 3

HCID 24611Copper bromide (CuBr2)触媒HCID 3283Diethyl Ether溶媒HCID 25517Ammonium Chloride溶媒

実験手順

To a solution in 500 ml of ether of 50.98 g of ethyl α-ethoxycarbonyl-o-bromo-cinnamate (170.5 mmole) and 1.0 g of copper bromide was added dropwise 56.7 ml of an ethereal solution of methylmagnesium bromide (175.6 mmole) at -20° C. The mixture was stirred overnight at room temperature, diluted with an aqueous ammonium chloride solution to separate the phases. The organic phase was dried over magnesium sulfate and concentrated under reduced pressure to give ethyl 3-(2-bromophenyl)-2-ethoxycarbonyl-3-methylpropionate.

後処理

  1. customto separate the phases
  2. dry with materialThe organic phase was dried over magnesium sulfate
  3. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-609869689b8d4703b7edca5bf824b63f
出典データセット
uspto-grants-1999_08
特許番号
US05942459

関連ノート

読み込み中…