反应详情

Thionyl chloride (54.6 g) was added dropwise at 40° C. to a solution of 3-(2,4-di-fluorophenyl)propionic acid (57 g) in methylene chloride (200 ml). After reaction was complete, excess thionyl chloride and the solvent were removed by distillation. The oily residue was added dropwise at 40° C. to a suspension of aluminium chloride (88.5 g) in methylene chloride (200 ml). The reaction mixture was added to dilute hydrochloric acid after 18 hours at 40° C. The aqueous phase was separated off and extracted once with methylene chloride (250 ml). The combined organic phases were freed from the solvent and then distilled in vacuo. 41 g of a colorless solid were obtained (m.p.: 103° C.).

1. customAfter reaction
2. customexcess thionyl chloride and the solvent were removed by distillation
3. additionThe oily residue was added dropwise at 40° C. to a suspension of aluminium chloride (88.5 g) in methylene chloride (200 ml)
4. additionThe reaction mixture was added to dilute hydrochloric acid after 18 hours at 40° C
5. customThe aqueous phase was separated off
6. extractionextracted once with methylene chloride (250 ml)
7. distillationdistilled in vacuo