反应详情

Anhydrous MgSO4 (3.4 g, 28 mmol) was suspended in DCM (28.1 mL) and to this vigorously stirred mixture was added concentrated sulfuric acid (0.7 g, 7 mmol). The resulting mixture was allowed to stir at ambient temperature for 30 minutes. 3-Oxocyclohexanecarboxylic acid (1.0 g, 7.0 mmol) was added followed by t-BuOH (2.6 g, 35 mmol). The resulting mixture was allowed to stir for 24 hours before it was filtered and flushed with DCM. The filtrate was washed with water, and the organic layer was again washed with water, brine, dried over anhydrous MgSO4, filtered, and concentrated in vacuo to afford the title compound. The residue was used without further purification.

1. stirringto stir for 24 hours before it
2. filtrationwas filtered
3. customflushed with DCM
4. washThe filtrate was washed with water
5. washthe organic layer was again washed with water, brine
6. dry with materialdried over anhydrous MgSO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo