Lithium hydroxide, monohydrate → 1-cyclopropyl-1H-pyrazole-3-carboxylic acid
반응식
[CH:1]1([N:4]2[CH:8]=[CH:7][C:6]([C:9]([O:11]C)=[O:10])=[N:5]2)[CH2:3][CH2:2]1.O[Li].O>C1COCC1.O>[CH:1]1([N:4]2[CH:8]=[CH:7][C:6]([C:9]([OH:11])=[O:10])=[N:5]2)[CH2:2][CH2:3]1참가 물질
5
실험 절차
Methyl 1-cyclopropyl-1H-pyrazole-3-carboxylate (2.5 g, 15 mmol) was dissolved in THF (40 ml) and H2O (10 ml). LiOH.H2O (1.50 g, 22.5 mmol) was added and the mixture was stirred at RT overnight. The reaction mixture was concentrated and acidified to pH 2 using 1 N HCl. The mixture was extracted with EtOAc and the organic layer was concentrated. Yield 1.6 g. 1H-NMR (400 MHz; DMSO-d6): δ 0.96-1.02 (m, 2H), 1.04-1.09 (m, 2H), 3.79-3.84 (m, 1H), 6.66 (d, 1H), 7.88 (d, 1H), 12.6 (bs, 1H).
후처리
- concentrationThe reaction mixture was concentrated
- extractionThe mixture was extracted with EtOAc
- concentrationthe organic layer was concentrated
출처 및 근거
- ORD 기록
- ord-87b6905f021b44f7a8db457a0f750b70
- 출처 데이터셋
- uspto-grants-2014_12
- 특허 번호
- US08921378B2
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