反应详情

A mixture of glyoxylic acid monohydrate (53.2 g, 578 mmol), acetic anhydride (530 mL, 5.61 mol) and acetic acid (120 mL) was refluxed for 2 h, concentrated in vacuo and azeotroped with toluene. The residue was diluted with toluene (270 mL), and thionyl chloride (84 mL, 1.15 mol) was added to the mixture. The resultant mixture was stirred at 60° C. for 16 h and concentrated in vacuo. The residue was purified by distillation (6-8 hpa, 70-80° C.) to afford compound the title compound as a colorless oil (70.7 g, 363 mmol, 63%).

1. temperaturewas refluxed for 2 h
2. concentrationconcentrated in vacuo
3. customazeotroped with toluene
4. additionwas added to the mixture
5. concentrationconcentrated in vacuo
6. distillationThe residue was purified by distillation (6-8 hpa, 70-80° C.)