Phosphorus oxychloride → HCID 88596891, compound

Participants

Reaction Conditions

Reaction Steps

Two 2000-mL 4-necked round-bottom flasks were charged with a solution of 15.3 (200 g, 718.58 mmol, 1.00 equiv) in POCl3 (2000 mL) at room temperature. The resulting solution was stirred for 2 h at 110° C. in an oil bath. The reaction mixture was cooled to room temperature and concentrated under vacuum. The reaction was then quenched by the addition of 1000 mL of ice-water. The resulting solution was extracted with 3×500 mL of ethyl acetate and the organic layers were combined. The combined organic layers were washed with 2×500 mL of brine, dried over anhydrous sodium sulfate and concentrated under vacuum to afford 200 g (94%) of ethyl 2-[12-chloro-7-thia-9,11-diazatricyclo[6.4.0.0^[2,6]]dodeca-1(12),2(6),8,10-tetraen-3-yl]acetate (15.4) as a light yellow solid.

Provenance & Evidence