Boron tribromide → HCID 19040960, 화합물

HRID 2399948노트

반응식

HRID 2399948 반응식
C[O:2][C:3]1[CH:20]=[C:19]([O:21]C)[CH:18]=[CH:17][C:4]=1[C:5]([N:7]([CH:14]([CH3:16])[CH3:15])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=[O:6].B(Br)(Br)Br>ClCCl>[OH:2][C:3]1[CH:20]=[C:19]([OH:21])[CH:18]=[CH:17][C:4]=1[C:5]([N:7]([CH:14]([CH3:16])[CH3:15])[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1)=[O:6]

참가 물질

4

반응물 2

HCID 25134Boron tribromideHCID 19040985HCID 19040985, 화합물

생성물 1

HCID 19040960HCID 19040960, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A stirred solution of 2,4-dimethoxy-N-(1-methylethyl)-N-phenylbenzamide (2.4 g, 8.03 mmol) in 10 ml of dichloromethane at 0° C. was treated with 1N boron tribromide (33.2 mL, 33.2 mmol) and stirred at room temperature for 1 hour. The reaction is poured in to the ice water. After stirring for 15 minutes, the reaction was partitioned between ethyl acetate and brine, dried over magnesium sulfate and concentrated in vacuo to afford yellow foam. This material is purified by chromatography on silica gel (70 g) with 3-5% methanol/dichloromethane as the eluent to afford 2,4-dihydroxy-N-(1-methylethyl)-N-phenylbenzamide as colorless foam.

후처리

  1. stirringAfter stirring for 15 minutes
  2. customthe reaction was partitioned between ethyl acetate and brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customto afford yellow foam
  6. customThis material is purified by chromatography on silica gel (70 g) with 3-5% methanol/dichloromethane as the eluent

출처 및 근거

ORD 기록
ord-07b264b656a64eaf925a6e38843ca29b
출처 데이터셋
uspto-grants-1995_09
특허 번호
US05451700

반응 노트

불러오는 중…