Carbon tetrabromide → 3-Bromomethyl-3-(3-hydroxy-phenyl)-1-methyl-azepan-2-one

HRID 1594892ノート

反応式

HRID 1594892 の反応式
O[CH2:2][C:3]1([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([OH:18])[CH:13]=2)[CH2:9][CH2:8][CH2:7][CH2:6][N:5]([CH3:10])[C:4]1=[O:11].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Br)(Br)(Br)[Br:39]>C(Cl)Cl>[Br:39][CH2:2][C:3]1([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([OH:18])[CH:13]=2)[CH2:9][CH2:8][CH2:7][CH2:6][N:5]([CH3:10])[C:4]1=[O:11]

参加物

5

反応物 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 217062823-Hydroxymethyl-3-(3-hydroxy-phenyl)-1-methyl-azepan-2-one

生成物 1

HCID 217061603-Bromomethyl-3-(3-hydroxy-phenyl)-1-methyl-azepan-2-one

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

3-Hydroxymethyl-3-(3-hydroxy-phenyl)-1-methyl-azepan-2-one (as described in Example 6, Step B) (0.60 g, 2.40 mmol), triphenylphosphine (0.94 g, 3.60 mmol), and carbon tetrabromide (1.19 g, 3.60 mmol) were dissolved in CH2Cl2 (15 mL), stirred under Ar for 16 h, then the solution was concentrated in vacuo and purified using SiO2 chromatography (0.5% MeOH/CH2Cl2) to give the title compound.

後処理

  1. concentrationthe solution was concentrated in vacuo
  2. custompurified

出典と根拠

ORDレコード
ord-8dbbe6964df940b1af33c2fd86d1a749
出典データセット
uspto-grants-2001_09
特許番号
US06284755B1

反応ノート

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