Ammonia → [1-Carbamoyl-4-(4-methoxy-phenyl)-butyl]-carbamic acid tert-butyl ester

HRID 1183030노트

반응식

HRID 1183030 반응식
C[O:2][C:3](=O)[CH:4]([NH:16][C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH2:5][CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=1.[NH3:25]>CO.O>[C:20]([O:19][C:17](=[O:18])[NH:16][CH:4]([C:3](=[O:2])[NH2:25])[CH2:5][CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=1)([CH3:23])([CH3:22])[CH3:21]

참가 물질

5

반응물 2

HCID 222AmmoniaHCID 669168592-tert-Butoxycarbonylamino-5-(4-methoxy-phenyl)-pentanoic acid methyl ester

생성물 1

HCID 66916855[1-Carbamoyl-4-(4-methoxy-phenyl)-butyl]-carbamic acid tert-butyl ester

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

A solution of 2-tert-butoxycarbonylamino-5-(4-methoxy-phenyl)-pentanoic acid methyl ester (5.6 g, 16.6 mmol) in MeOH (100 mL) is treated with aqueous ammonia solution (100 mL of a 28% solution in water, 28 mmol) and stirred at RT overnight. The organic solvent is removed in vacuo and the remaining aqueous portion is extracted with EtOAc (×3). The combined organic extracts are washed with brine and then dried (MgSO4) and concentrated in vacuo to afford the title compound as a yellow oil.

후처리

  1. customThe organic solvent is removed in vacuo
  2. extractionthe remaining aqueous portion is extracted with EtOAc (×3)
  3. washThe combined organic extracts are washed with brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-669057166c2844788a277453b92540b6
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08664228B2

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