反应 #1328423

ord-b19f7c0f445b4027a7c44e809fcc3001

反应方程式

COC(=O)c1ccc(Cl)c2c1SCCC2=O
methyl 5-chloro-4-oxothiochromane-8-carboxylate
COC(OC)N(C)C
N,N-dimethylformamide dimethyl acetal
COC(=O)c1ccc(Cl)c2c1SCC(=CN(C)C)C2=O
methyl 5-chloro-3-(N,N-dimethylaminomethylidene)-4-oxothiochromane-8-carboxylate
收率 97.0%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.DISTILLATIONVolatile components were then distilled off
  2. 2
    洗涤the organic phase was washed with water
  3. 3
    其他Drying
  4. 4
    其他removal of the solvent

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07115545B1uspto-grants-2006_10