Lithium hydroxide, monohydrate → 1-cyclopropyl-1H-pyrazole-3-carboxylic acid
反応式
[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]1参加物
5
実験手順
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).
後処理
- concentrationThe reaction mixture was concentrated
- extractionThe mixture was extracted with EtOAc
- concentrationthe organic layer was concentrated
出典と根拠
- ORDレコード
- ord-87b6905f021b44f7a8db457a0f750b70
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08921378B2
反応ノート
読み込み中…