反应详情

To a 500 mL three-opening flask were added 2,2-diphenylacetic acid (20 g, 94 mmol) and 200 mL dichloromethane. After stirring, 1 mL DMF was added. To the mixture was slowly added oxalyl chloride (13.16 g, 104 mmol) dropwisely in an ice bath. The reaction was conducted at 25° C. After the completion of reaction, the mixture was evaporated under reduced pressure to remove oxalyl chloride. To the reaction flask were slowly added dichloromethane (100 mL) and anhydrous methanol (3.61 g, 113 mmol) dropwisely under cooling in an ice bath respectively. The reaction was conducted at 25° C. After the completion of reaction, the reaction solution was washed with a saturated aqueous NaCl solution. The organic phase was dried over sodium sulfate, and filtered by suction. The filtrate was evaporated to dryness to produce methyl 2,2-diphenylacetate (21 g) in a yield of 98.7%.

1. customwas conducted at 25° C
2. customAfter the completion of reaction
3. customthe mixture was evaporated under reduced pressure
4. customto remove oxalyl chloride
5. temperatureunder cooling in an ice bath respectively
6. customwas conducted at 25° C
7. customAfter the completion of reaction
8. washthe reaction solution was washed with a saturated aqueous NaCl solution
9. dry with materialThe organic phase was dried over sodium sulfate
10. filtrationfiltered by suction
11. customThe filtrate was evaporated to dryness