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

HRID 1594892노트

반응식

HRID 1594892 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  1. concentrationthe solution was concentrated in vacuo
  2. custompurified

출처 및 근거

ORD 기록
ord-8dbbe6964df940b1af33c2fd86d1a749
출처 데이터셋
uspto-grants-2001_09
특허 번호
US06284755B1

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