Boron tribromide → HCID 178434358, 화합물

HRID 380436노트

반응식

HRID 380436 반응식
C[O:2][C:3]1[CH:11]=[C:10]2[C:6]([C:7]([CH3:12])=[N:8][NH:9]2)=[CH:5][CH:4]=1.B(Br)(Br)Br>ClCCl>[OH:2][C:3]1[CH:11]=[C:10]2[C:6]([C:7]([CH3:12])=[N:8][NH:9]2)=[CH:5][CH:4]=1

참가 물질

4

반응물 2

HCID 25134Boron tribromideHCID 178487565HCID 178487565, 화합물

생성물 1

HCID 178434358HCID 178434358, 화합물수율 93%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 6-methoxy-3-methyl-1 H-indazole(2.0 g, Reference Example 49) in dichloromethane (75 ml) was cooled to 0° C. then treated with a solution of boron tribromide in dichloromethane (54 ml, 1M). The mixture was allowed to warm to room temperature and then stirred for 12 hours. The solution was poured into an ice-saturated sodium bicarbonate mixture and the aqueous layer was extracted three times with ethyl acetate (50 ml). The combined extracts were dried over sodium sulphate then evaporated. The residue was subjected to flash chromatography on silica eluting with a mixture of ethyl acetate and hexane (2:1, v/v) to yield the title compound (1.7 g).

후처리

  1. extractionthe aqueous layer was extracted three times with ethyl acetate (50 ml)
  2. dry with materialThe combined extracts were dried over sodium sulphate
  3. customthen evaporated
  4. additionThe residue was subjected to flash chromatography on silica eluting with a mixture of ethyl acetate and hexane (2:1

출처 및 근거

ORD 기록
ord-cbdda4033d794759bb50c2a1e457cf72
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06303600B1

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