反应详情

Trifluoroacetic acid (50 mL, 0.073 mol) was added dropwise to a stirred mixture of (tert-Butoxycarbonylimino-thiomorpholin-4-yl-methyl)-carbamic acid tert-butyl ester (21 g, 0.0723 mol) in DCM (200 mL) and water (10 mL). After 3 days at rt, the solvent was evaporated and re-evaporated with 2-propanol. The resulting semi-solid was triturated with 10% 2-propanol/Et2O. The solid was filtered off and was washed with 10% 2-propanol/Et2O and then with Et2O. The product was dried in vacuo over phosphoric oxide, to give 15.72 g as a white solid.

1. customthe solvent was evaporated
2. customre-evaporated with 2-propanol
3. customThe resulting semi-solid was triturated with 10% 2-propanol/Et2O
4. filtrationThe solid was filtered off
5. washwas washed with 10% 2-propanol/Et2O
6. dry with materialThe product was dried in vacuo over phosphoric oxide
7. customto give 15.72 g as a white solid