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

HRID 275850
ノート
印刷プレビュー

反応式

HRID 275850 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4da33944a177480fbea22546decfe0d8
出典データセット
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06352982B1

反応ノート

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