反应详情

温度

0 °C

A 100 mL round bottom flask was charged with 319 (0.55 g, 1.3 mmol) and DIPEA (0.91 mL, 5.2 mmol) in dry tetrahydrofuran (55 mL) to give a colorless solution. The reaction mixture was cooled to 0° C. then triphosgene (0.154 g, 0.520 mmol) was added. The reaction mixture was stirred for 1 h at 0° C. then cyclopropylamine (1.8 mL, 26 mmol) was added. Finally the reaction mixture was stirred at r.t. for 3 h then concentrated. The residue was partitioned between water and ethyl acetate, resulting in the formation a thick white solid. This was isolated by suction filtration, rinsed with water and ethyl acetate, and dried in vacuo to give crude 320 (0.65 g, 1.2 mmol, 99% yield) which was used without further purification. MS: 507.2 (M+H).

1. customto give a colorless solution
2. stirringFinally the reaction mixture was stirred at r.t. for 3 h
3. concentrationthen concentrated
4. customThe residue was partitioned between water and ethyl acetate
5. customresulting in the formation a thick white solid
6. customThis was isolated by suction filtration
7. washrinsed with water and ethyl acetate
8. customdried in vacuo