Dibenzylamine → Ethyl 4-(Dibenzylamino)butanoate

HRID 129925ノート

反応式

HRID 129925 の反応式
I[CH2:2][CH2:3][CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].[CH2:10]([NH:17][CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[CH2:18]([N:17]([CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[CH2:2][CH2:3][CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1

参加物

5

反応物 3

HCID 7656DibenzylamineHCID 11430Potassium CarbonateHCID 10890062Ethyl 4-iodobutanoate

生成物 1

HCID 13929784Ethyl 4-(Dibenzylamino)butanoate収率 83.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Mix ethyl 4-iodobutyrate (43.5 g, 0.18 mol), dibenzylamine (35.5 g, 0.18 mol), potassium carbonate (24.9 g, 0.18 mol) and ethanol (114 mL dried over 4A molecular sieves). Reflux for 24 hours then stir at room temperature for 48 hours. Add methylene chloride (100 mL) and filter. Evaporate the filtrate to a residue and purify by silica gel chromatography (methylene chloride) to give the title compound (47 g).

後処理

  1. temperatureReflux for 24 hours
  2. filtrationAdd methylene chloride (100 mL) and filter
  3. customEvaporate the filtrate to a residue
  4. custompurify by silica gel chromatography (methylene chloride)

出典と根拠

ORDレコード
ord-4178cabbe3c14fa8aa1780a21d3129cc
出典データセット
uspto-grants-1995_11
特許番号
US05470844

反応ノート

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