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Methanol → 2-Amino-5-chloro-alpha-(4-tert-butoxycarbonylaminomethylphenyl)benzyl alcohol

HRID 275850
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HRID 275850 반응식
CO.[NH2:3][C:4]1[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][C:5]=1[C:6]([C:8]1[CH:13]=[CH:12][C:11]([CH2:14][NH:15][C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])=[CH:10][CH:9]=1)=[O:7].[BH4-].[Na+]>C(OC(=O)C)C>[NH2:3][C:4]1[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][C:5]=1[CH:6]([OH:7])[C:8]1[CH:13]=[CH:12][C:11]([CH2:14][NH:15][C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])=[CH:10][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 4311764Sodium borohydrideHCID 183153642-Amino-4'-tert-butoxycarbonylaminomethyl-5-chlorobenzophenone

생성물 1

HCID 545021332-Amino-5-chloro-alpha-(4-tert-butoxycarbonylaminomethylphenyl)benzyl alcohol수율 93.9%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a methanol (10 ml) solution of 2-amino-4′-tert-butoxycarbonylaminomethyl-5-chlorobenzophenone (0.9 g) was added sodium borohydride (0.28 g). The mixture was stirred for 30 minutes at room temperature, to which was added acetic acid ethyl ester (100 ml). The mixture was washed with water and dried over anhydrous Na2SO4. The solvent was then distilled off, and the residue was purified by means of a silica gel column chromatography to give the object 2-amino-5-chloro-α-(4-tert-butoxycarbonylaminomethylphenyl)benzyl alcohol (0.85 g) as a colorless oily product.

후처리

  1. washThe mixture was washed with water
  2. dry with materialdried over anhydrous Na2SO4
  3. distillationThe solvent was then distilled off
  4. customthe residue was purified by means of a silica gel column chromatography

출처 및 근거

ORD 기록
ord-4da33944a177480fbea22546decfe0d8
출처 데이터셋
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06352982B1

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