Sodium Hydroxide → 1H-Indazol-5-ol
반응식
C[O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[NH:8][N:7]=[CH:6]2.B(Br)(Br)Br.[OH-].[Na+]>C(Cl)CCl.C(Cl)Cl>[OH:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[NH:8][N:7]=[CH:6]2참가 물질
6
실험 절차
5-Methoxyindazole (1.7 g, 11.5 mmol), (Tetrahedron, 1994, 50, 3529), was dissolved in ethylene chloride (35 ml) and cooled in an ice/water bath. Boron tribromide (57.4 ml of a 1M olution in methylene chloride, 57.4 mmol) was added over 10 minutes and then the mixture allowed to warm to ambient temperature. The mixture was stirred for 2 hours and then re-cooled in an ice/water bath. 2N Sodium hydroxide was slowly added until pH 8. The precipitated solid was filtered off and dried under vacuum at 60° C. overnight. The residue was purified by column chromatography eluting with methylene chloride/methanol (95/5) to give 5-hydroxyindazole (1.0 g, 65%) as a brown solid.
후처리
- temperaturecooled in an ice/water bath
- temperaturere-cooled in an ice/water bath
- filtrationThe precipitated solid was filtered off
- customdried under vacuum at 60° C. overnight
- customThe residue was purified by column chromatography
- washeluting with methylene chloride/methanol (95/5)
출처 및 근거
- ORD 기록
- ord-0deb1d7ed7794615898ae5d85b81ecde
- 출처 데이터셋
- uspto-grants-2007_09
- 특허 번호
- US07268230B2
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