Sodium Acetate → 1,5‐Dimethyl‐6‐sulfanylidene‐3‐(2,2,7‐trifluoro‐3‐ oxo‐3,4‐dihydro‐2H‐1,4‐benzoxazin‐6‐yl)‐1,3,5‐ triazinane‐2,4‐dione

Participants

Reaction Conditions

Reaction Steps

0.97 g (5.0 mmol) methyl N-methyl-N-(methylcarbamothioyl)carbamate with a purity of 83.3% was dissolved in 4.2 g DMF. 0.14 g (1.7 mmol) sodium acetate was added. The mixture was stirred at 60° C. at a pressure of 25 mbar. Via syringe a solution of 1.32 g (3.7 mmol) phenyl N-(2,2,7-trifluoro-3-oxo-3,4-dihydro-2H-benzo[b][1,4]oxazin-6-yl)carbamate (purity 95.7%) in 4.2 g DMF was added within 2 h. From time to time fresh DMF was added to maintain the solvent volume. After a poststirring period of 1 h, a chemical yield 73% was determined by quantitative HPLC analytics (HPLC-method A; tR=4.9 min) of the product solution.

Provenance & Evidence