反应详情

Thiophosgene (33.6 g) in CHCl3 (250 ml) and K2CO3 (64.7 g) in H2O (450 ml) are added, separately and simultaneously, drop wise to a solution of 3-tert-Butoxy-5-fluoro-phenyl-amine (42.9 g) in CHCl3 (350 ml) at 0° C. The reaction mixture is warmed to room temperature over night. The organics are separated and washed with water (3×), brine (1×), dried over MgSO4, filtered and the solvent removed in vacuo. The title compound is obtained by flash column chromatography (silica, eluent dichloromethane/iso-hexane 1:3). 1H nmr (CDCl3, 400 MHz); 6.70 (m, 3H), 1.40 (s, 9H).

1. customThe organics are separated
2. washwashed with water (3×), brine (1×)
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. customthe solvent removed in vacuo