1-Butanol → Diphenylacetyl-carbamic acid butyl ester

HRID 392686

반응식

HRID 392686 반응식
[CH2:1]([OH:5])[CH2:2][CH2:3][CH3:4].[C:6]1([CH:12]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:13]([N:15]=[C:16]=[O:17])=[O:14])[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1>ClCCl>[CH2:1]([O:5][C:16](=[O:17])[NH:15][C:13](=[O:14])[CH:12]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[CH2:2][CH2:3][CH3:4]

참가 물질

4

반응물 2

HCID 2631-ButanolHCID 11264874Diphenylacetyl isocyanate

생성물 1

HCID 9883204Diphenylacetyl-carbamic acid butyl ester수율 83.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirred solution of 1-butanol (0.32 ml, 3.49 mmol) in dichloromethane (4 ml) was added a solution of diphenylacetyl isocyanate (2.33 ml, 0.5M in CH2Cl2, 1.16 mmol) and the mixture was stirred at RT for 1 h. Removal of the solvent in vacuum left a yellow oil, which was purified by column chromatography on silica gel (ethyl acetate/hexane 1:2) to give the title compound (0.3 g, 83%) as a light yellow solid, m.p. 82-84° C. and MS: m/e=334 (M+Na+).

후처리

  1. customRemoval of the solvent in vacuum
  2. waitleft a yellow oil, which
  3. customwas purified by column chromatography on silica gel (ethyl acetate/hexane 1:2)

출처 및 근거

ORD 기록
ord-c63e3bc3941d4ebd8d04e15890bd6770
출처 데이터셋
uspto-grants-2004_10
특허 번호
US06803381B1

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