Thiophosgene → HCID 52914145, compound

Participants

Reaction Steps

A solution of compound 28 (1.21 g, 1.75 mmol) in 0.5 M HCl (50 mL) was carefully added to thiophosgene (CSCl2) (4.03 mL, 6.04 g, 52.5 mmol) in CHCl3 (50 mL). The reaction mixture was stirred for 5 hours at room temperature and the layers were allowed to separate. The aqueous layer was removed and the organic CHCl3 layer was then washed with water (2×50 mL). The combined aqueous layers were washed with CHCl3 (3×50 mL) to remove unreacted thiophosgene. Finally, the aqueous layer was lyophilized to afford white crystalline solid 29 (1.26 g, 98% yield).

Provenance & Evidence