Methanol → 2-Amino-5-chloro-alpha-[4-(2-tert-butoxycarbonylaminoethyl)phenyl]benzyl alcohol

HRID 275853ノート

反応式

HRID 275853 の反応式
CO.[NH2:3][C:4]1[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][C:5]=1[C:6]([C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][NH:16][C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])=[CH:10][CH:9]=1)=[O:7].[BH4-].[Na+]>C(OC(=O)C)C>[NH2:3][C:4]1[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][C:5]=1[CH:6]([OH:7])[C:8]1[CH:9]=[CH:10][C:11]([CH2:14][CH2:15][NH:16][C:17]([O:19][C:20]([CH3:23])([CH3:21])[CH3:22])=[O:18])=[CH:12][CH:13]=1

参加物

5

反応物 3

HCID 887MethanolHCID 4311764Sodium borohydrideHCID 183153782-Amino-4'-(2-tert-butoxycarbonylaminoethyl)-5-chlorobenzophenone

生成物 1

HCID 696967742-Amino-5-chloro-alpha-[4-(2-tert-butoxycarbonylaminoethyl)phenyl]benzyl alcohol収率 109.4%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a methanol (40 ml) solution of 2-amino-4′-(2-tert-butoxycarbonylaminoethyl)-5-chlorobenzophenone (2.0 g) was added sodium borohydride (0.5 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, then, dried over anhydrous MgSO4, followed by distilling off the solvent. The residue was purified by means of a silica gel column chromatography to give the object 2-amino-5-chloro-α-[4-(2-tert-butoxycarbonylaminoethyl)phenyl]benzyl alcohol (2.2 g) as a colorless oily product.

後処理

  1. washThe mixture was washed with water
  2. dry with materialdried over anhydrous MgSO4
  3. distillationby distilling off the solvent
  4. customThe residue was purified by means of a silica gel column chromatography

出典と根拠

ORDレコード
ord-3adf72da0be14c7887c69b66cc2df0cc
出典データセット
uspto-grants-2002_03
特許番号
US06352982B1

反応ノート

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