反应详情

温度

0 °C

In a round-bottomed flask, ((1R,3R)-3-carbamoyl-cyclopentyl)-carbamic acid tert-butyl ester (96 mg, 0.42 mmol) was suspended in THF (2.5 ml). The reaction mixture was cooled to 0° C. and triethylamine (0.28 ml, 2.01 mmol) followed by trifluoroacetic anhydride (0.095 ml, 0.67 mmol) were added. The homogeneous reaction mixture was stirred at 0° C. for 1.5 h then quenched with water and extracted with dichloromethane (2×). The combined organic layers were dried over sodium sulfate, filtered and concentrated to afford ((1R,3R)-3-cyanocyclopentyl)-carbamic acid tert-butyl ester as an off-white waxy solid which contained some triethylamine trifluoroacetate as a major impurity. This material was used without further purification.

1. additionwere added
2. customthen quenched with water
3. extractionextracted with dichloromethane (2×)
4. dry with materialThe combined organic layers were dried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated