反応 #1328423
ord-b19f7c0f445b4027a7c44e809fcc3001
反応方程式
methyl 5-chloro-4-oxothiochromane-8-carboxylate
N,N-dimethylformamide dimethyl acetal
→
methyl 5-chloro-3-(N,N-dimethylaminomethylidene)-4-oxothiochromane-8-carboxylate
収率 97.0%
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1workup.DISTILLATIONVolatile components were then distilled off
- 2洗浄the organic phase was washed with water
- 3その他Drying
- 4その他removal of the solvent
実験手順
30 g (0.078 mol) of methyl 5-chloro-4-oxothiochromane-8-carboxylate in 300 ml of N,N-dimethylformamide dimethyl acetal were refluxed for 6 hours. Volatile components were then distilled off, the residue was taken up in methylene chloride and the organic phase was washed with water. Drying and removal of the solvent gave 35.3 g (97%) of methyl 5-chloro-3-(N,N-dimethylaminomethylidene)-4-oxothiochromane-8-carboxylate.