Boron tribromide → HCID 23499550, 화합물

HRID 1836425노트

반응식

HRID 1836425 반응식
B(Br)(Br)Br.C[O:6][C:7]1[CH:15]=[CH:14][C:10]([C:11]([OH:13])=[O:12])=[C:9]([C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=2)[CH:8]=1>ClCCl>[OH:6][C:7]1[CH:15]=[CH:14][C:10]([C:11]([OH:13])=[O:12])=[C:9]([C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=2)[CH:8]=1

참가 물질

4

반응물 2

HCID 25134Boron tribromideHCID 23499547HCID 23499547, 화합물

생성물 1

HCID 23499550HCID 23499550, 화합물수율 62%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

A solution of boron tribromide in dichloromethane (1M, 66 ml.) was added dropwise to a stirred solution of 4-methoxy-2-(4-fluorophenyl)benzoic acid (7.7 g.) in dried dichloromethane (215 ml) under an argon atmosphere at 0° C. The reaction was stirred for 1 hour at 0° C., allowed to warm to ambient temperature and stirred for 16 hours. The reaction was poured into ice water and extracted with dichloromethane followed by ethyl acetate. The combined organic extracts were washed with saturated aqueous sodium hydrogen carbonate and the aqueous phase acidified to pH 1 with concentrated hydrochloric acid and extracted with ethyl acetate. The ethyl acetate extracts were dried and evaporated to dryness to give 4-hydroxy-2-(4-fluorophenyl)benzoic acid (Compound xxx) as a yellow oil (4.5 g), which was used without further purification.

후처리

  1. temperatureto warm to ambient temperature
  2. stirringstirred for 16 hours
  3. extractionextracted with dichloromethane
  4. washThe combined organic extracts were washed with saturated aqueous sodium hydrogen carbonate
  5. extractionextracted with ethyl acetate
  6. dry with materialThe ethyl acetate extracts were dried
  7. customevaporated to dryness

출처 및 근거

ORD 기록
ord-dc97306edac84c7e97ba3de359031ebc
출처 데이터셋
uspto-grants-2004_08
특허 번호
US06777438B2

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