4-Methylmorpholine → 4,4-Difluorocyclohexanecarboxamide
反応式
[F:1][C:2]1([F:11])[CH2:7][CH2:6][CH:5]([C:8](O)=[O:9])[CH2:4][CH2:3]1.C[N:13]1CCOCC1.CC(COC(Cl)=O)C.[OH-].[NH4+]>C1COCC1>[F:1][C:2]1([F:11])[CH2:7][CH2:6][CH:5]([C:8]([NH2:13])=[O:9])[CH2:4][CH2:3]1参加物
6
反応条件
- 温度
- 0 °C
実験手順
To a solution of compound 4,4-difluorocyclohexanecarboxylic acid (3.5 g, 21 mmol) in 80 mL THF, 4-methylmorpholine (2.51 g, 21 mmol) was added at −70° C., followed by isobutyl chloridocarbonate (2.85 g, 21 mmol). 30 min later, 10 mL ammonium hydroxide was added. The resulting mixture was allowed to warm up to 0° C. After removal of all solvents, the residue was washed with water, PE to afford the compound 4,4-difluorocyclohexanecarboxamide (1.82 g, 40%) as a white solid.
後処理
- customAfter removal of all solvents
- washthe residue was washed with water, PE
出典と根拠
- ORDレコード
- ord-2174b11f6a2345ac992642fda24bab23
- 出典データセット
- uspto-grants-2016_08
- 特許番号
- US09416132B2
反応ノート
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