Trifluoroacetic acid → 3-Bromo-1H-pyrrolo[3,2-c]pyridin-4-ol
반응식
[Br:1][C:2]1[C:6]2[C:7](=[O:11])[NH:8][CH:9]=[CH:10][C:5]=2[N:4](COCC[Si](C)(C)C)[CH:3]=1.C([SiH](CC)CC)C.FC(F)(F)C(O)=O>>[Br:1][C:2]1[C:6]2[C:7](=[O:11])[NH:8][CH:9]=[CH:10][C:5]=2[NH:4][CH:3]=1참가 물질
4
실험 절차
To a suspension of 3-bromo-1-((2-(trimethylsilyl)ethoxy)methyl)-1,5-dihydro-4H-pyrrolo[3,2-c]pyridin-4-one (2.0 g) and triethylsilane (1.27 g) was added trifluoroacetic acid (17.31 mL) at room temperature, and the mixture was stirred under nitrogen atmosphere at room temperature for 1 hr. The reaction mixture was concentrated under reduced pressure, to the residue were added acetonitrile (11 mL) and aqueous ammonia solution (25%, 11 mL), and the mixture was stirred at room temperature for 2 hr. The precipitate was collected by filtration, and washed with acetonitrile and ethyl acetate to give the title compound (1.06 g).
후처리
- concentrationThe reaction mixture was concentrated under reduced pressure, to the residue
- additionwere added acetonitrile (11 mL) and aqueous ammonia solution (25%, 11 mL)
- stirringthe mixture was stirred at room temperature for 2 hr
- filtrationThe precipitate was collected by filtration
- washwashed with acetonitrile and ethyl acetate
출처 및 근거
- ORD 기록
- ord-40c8cf6c8469448f907809f43b2f1a7e
- 출처 데이터셋
- uspto-grants-2016_06
- 특허 번호
- US09371320B2
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