Diethyl (ethoxymethylene)malonate → HCID 59255053、化合物

HRID 639537ノート

反応式

HRID 639537 の反応式
[CH:1]([N:4]=[C:5]([CH3:7])[CH3:6])([CH3:3])[CH3:2].[CH2:8]([O:10][C:11](=[O:22])[C:12](=[CH:18]OCC)[C:13](OCC)=[O:14])[CH3:9]>C1(OC2C=CC=CC=2)C=CC=CC=1>[CH:5]([N:4]1[C:1]([CH3:3])=[CH:2][CH:18]=[C:12]([C:11]([O:10][CH2:8][CH3:9])=[O:22])[C:13]1=[O:14])([CH3:7])[CH3:6]

参加物

4

反応物 2

HCID 6871Diethyl (ethoxymethylene)malonateHCID 1378922-Propanamine, N-(1-methylethylidene)-

生成物 1

HCID 59255053HCID 59255053、化合物収率 70%

試薬・触媒・溶媒 1

HCID 7583Diphenyl Ether溶媒

反応条件

温度
185 °C

実験手順

A mixture of isopropyl(1-methylethylidene)amine (7.94 g, 80.0 mmol, prepared according to Newcomb, Martin et al., J. Amer. Chem. Soc., 1990, 112, 5186) and diethyl(ethoxymethylene)malonate (17.31 g, 80.0 mmol) in diphenyl ether (48 mL) was stirred in a sealed tube at 180-190° C. for 18 h. After cooling, the mixture was chromatographed on a column of silica gel eluting with n-hexane/ethyl acetate (v/v=1/1˜1/2) to give 12.5 g (70%) of the title compound as brown oil.

後処理

  1. temperatureAfter cooling
  2. customthe mixture was chromatographed on a column of silica gel eluting with n-hexane/ethyl acetate (v/v=1/1˜1/2)

出典と根拠

ORDレコード
ord-fff9c7399a8a4d669d53c55ae152a755
出典データセット
uspto-grants-2010_04
特許番号
US07691881B2

反応ノート

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