反应详情

A mixture of EXAMPLE 385A (475 mg) and potassium hydroxide (641 mg) in toluene (10 mL) and water (25 mL) was cooled in an ice bath and phosgene (20% in toluene, 2.178 mL) was added dropwise maintaining the temperature below 3° C. The reaction was stirred rapidly at ambient temperature for 3 hours while warming to ambient temperature. The reaction mixture was partitioned between brine (100 mL) and ethyl acetate (100 mL). The organics were dried over sodium sulfate, filtered, and concentrated to provide the title compound.

1. temperaturemaintaining the temperature below 3° C
2. temperaturewhile warming to ambient temperature
3. customThe reaction mixture was partitioned between brine (100 mL) and ethyl acetate (100 mL)
4. dry with materialThe organics were dried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated