Benzyl N-(4-aminobutyl)carbamate → Ethyl 2-(4-benzyloxycarbonylaminobutyl)aminomethyl-4-phenylbutyrate

HRID 978429ノート

反応式

HRID 978429 の反応式
[CH2:1]([O:8][C:9]([NH:11][CH2:12][CH2:13][CH2:14][CH2:15][NH2:16])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:17]([C:25](=[CH2:31])[C:26]([O:28][CH2:29][CH3:30])=[O:27])[CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>C(O)C>[CH2:1]([O:8][C:9]([NH:11][CH2:12][CH2:13][CH2:14][CH2:15][NH:16][CH2:31][CH:25]([CH2:17][CH2:18][C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1)[C:26]([O:28][CH2:29][CH3:30])=[O:27])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 2783677Benzyl N-(4-aminobutyl)carbamateHCID 11117162Ethyl alpha-(phenethyl)acrylate

生成物 1

HCID 20203289Ethyl 2-(4-benzyloxycarbonylaminobutyl)aminomethyl-4-phenylbutyrate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 20 g of 4-benzyloxycarbonylamino-1-butylamine, 21.04 g of ethyl α-(phenethyl)acrylate and 200 ml of ethanol was stirred at room temperature for 8 days and evaporated to dryness. The residue was dissolved in ethyl ether and the solution was extracted three times with 100 ml of 2N hydrochloric acid. The aqueous layer was basified with 2N sodium hydroxide and extracted three times with methylene chloride, dried over magnesium sulfate and evaporated to give the ethyl 2-(4-benzyloxycarbonylaminobutyl)aminomethyl-4-phenylbutyrate having signals in the NMR spectrum at δ=7.4, 7.25, and 5.1 ppm.

後処理

  1. customevaporated to dryness
  2. dissolutionThe residue was dissolved in ethyl ether
  3. extractionthe solution was extracted three times with 100 ml of 2N hydrochloric acid
  4. extractionextracted three times with methylene chloride
  5. dry with materialdried over magnesium sulfate
  6. customevaporated

出典と根拠

ORDレコード
ord-9c2338b2512946f8b623353ee77a3dfe
出典データセット
uspto-grants-1987_05
特許番号
US04665087

反応ノート

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