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

HRID 275844
ノート
印刷プレビュー

反応式

HRID 275844 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][CH:11]=[CH:10][C:9]=1[CH2:14][NH:15][C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])=[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][CH:11]=[CH:10][C:9]=1[CH2:14][NH:15][C:16]([O:18][C:19]([CH3:20])([CH3:21])[CH3:22])=[O:17]
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 183153772-Amino-2'-tert-butoxycarbonylaminomethyl-5-chlorobenzophenone

生成物 1

HCID 539893822-Amino-5-chloro-alpha-(2-tert-butoxycarbonylaminomethylphenyl)benzyl alcohol収率 99.4%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a methanol (5 ml) solution of 2-amino-2′-tert-butoxycarbonylaminomethyl-5-chlorobenzophenone (0.5 g) was added sodium borohydride (79 mg). The mixture was stirred for 3 hours at room temperature. To the reaction mixture was added acetic acid ethyl ester (100 ml), which was washed with water and, then, dried over anhydrous MgSO4. The solvent was distilled off, and the residue was purified by means of a silica gel column chromatography to give the object 2-amino-5-chloro-α-(2-tert-butoxycarbonylaminomethylphenyl)benzyl alcohol (0.5 g) as a colorless oily product.

後処理

  1. washwas washed with water
  2. dry with materialdried over anhydrous MgSO4
  3. distillationThe solvent was 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-fb242133f4ca4d78ba15ec50d239e3ba
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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このページの内容参加物実験手順後処理出典と根拠反応ノート