反应详情

To a suspension of 2-(2-isopropyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulene-9-sulfonic acid (228 mg, 0.61 mmol) in THF (15 mL) was added oxalyl chloride (257 μL, 3.04 mmol) and the resulting mixture stirred at RT for 15 min. The reaction mixture was cooled to 0° before DMF (126 μL, 1.69 mmol) was added and the resulting mixture warmed to RT after 10 min then stirred for a further 2 h. The reaction mixture was azeotroped with toluene affording 2-(2-Isopropyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulene-9-sulfonyl chloride (500 mg).

1. additionwas added
2. temperaturethe resulting mixture warmed to RT after 10 min
3. stirringthen stirred for a further 2 h
4. customThe reaction mixture was azeotroped with toluene