Sodium Hydroxide → 4,5,6,7-Tetrahydro-1H-indazole-3-carboxylic acid
반응식
C([O:3][C:4]([C:6]1[C:14]2[CH2:13][CH2:12][CH2:11][CH2:10][C:9]=2[NH:8][N:7]=1)=[O:5])C.[OH-].[Na+]>CO>[NH:8]1[C:9]2[CH2:10][CH2:11][CH2:12][CH2:13][C:14]=2[C:6]([C:4]([OH:5])=[O:3])=[N:7]1참가 물질
4
실험 절차
A solution of 4,5,6,7-tetrahydro-1H-indazole-3-carboxylic acid ethyl ester [0.606 g, Reference Example 18(a)] in methanol (50 ml) was treated with sodium hydroxide (0.500 g). The mixture was refluxed for 16 hours, then cooled and then evaporated. The residual white solid was treated with hydrochloric acid (30 ml, 2N) and the resulting solution was extracted three times with ethyl acetate (50 ml). The combined organic extracts were dried over sodium sulfate and then evaporated to yield 4,5,6,7-tetrahydro-1H-indazole-3-carboxylic acid (0.424 g) as a white solid. LC-MS (METHOD B): RT=2.44 minutes; 167 (M+H)+.
후처리
- temperatureThe mixture was refluxed for 16 hours
- temperaturecooled
- customevaporated
- additionThe residual white solid was treated with hydrochloric acid (30 ml, 2N)
- extractionthe resulting solution was extracted three times with ethyl acetate (50 ml)
- dry with materialThe combined organic extracts were dried over sodium sulfate
- customevaporated
출처 및 근거
- ORD 기록
- ord-b50ccbe39e3a45fdb4929b6ff99e8427
- 출처 데이터셋
- uspto-grants-2012_10
- 특허 번호
- US08288425B2
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