Water → Ethyl (4,4-diethoxybutyl)carbamate

HRID 1418367

反応式

HRID 1418367 の反応式
Cl[C:2]([O:4][CH2:5][CH3:6])=[O:3].[CH2:7]([O:9][CH:10]([O:15][CH2:16][CH3:17])[CH2:11][CH2:12][CH2:13][NH2:14])[CH3:8].N1C=CC=CC=1.O>ClCCl>[CH2:16]([O:15][CH:10]([O:9][CH2:7][CH3:8])[CH2:11][CH2:12][CH2:13][NH:14][C:2](=[O:3])[O:4][CH2:5][CH3:6])[CH3:17]

参加物

6

反応物 4

HCID 962WaterHCID 1049PyridineHCID 10928Ethyl chloroformateHCID 806724,4-Diethoxybutylamine

生成物 1

HCID 54057192Ethyl (4,4-diethoxybutyl)carbamate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Ethyl chloroformate (0.3 ml, 3.1 mmol) was added dropwise to a solution of 4-aminobutanal diethyl acetal (0.5 ml, 2.9 mmol) and pyridine (0.28 ml, 3.5 mmol) in dichloromethane (10 ml) at 5° C. The mixture was stirred for 30 min. Water was added and the mixture was extracted with ether. The ether was dried (sodium sulphate) and evaporated to give the product as a yellow oil, MS (+EI) 232 ([M-H]+), 1H NMR (CDCl3) 4.69 (1H, s), 4.4 (1H, t), 4.00 (2H, q), 3.5-3.65 (2H, m), 3.35-3.5 (2H, m), 3.05-3.15 (2H, m), 1.5-1.6 (4H, m), 1.1-1.2 (9H, m).

後処理

  1. extractionthe mixture was extracted with ether
  2. dry with materialThe ether was dried (sodium sulphate)
  3. customevaporated

出典と根拠

ORDレコード
ord-1a4c542dd1ec4e3783b3f746f0d78c9b
出典データセット
uspto-grants-1999_03
特許番号
US05883102

関連ノート

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