反应 #1050686

ord-222a53e0fd964792a3b3be06146c9e16

反应方程式

CCOC(C)=O
ethyl acetate
Cc1ccc(S(=O)(=O)O)cc1
p-toluene-sulfonic acid
Cc1ccc(C=O)s1
2-formyl-5-methylthiophene
COC([O-])[O-]
methyl orthoformate
COC(OC)c1ccc(C)s1
2-dimethoxymethyl-5-methylthiophene
收率 78.5%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他To the cooled reaction mixture
  2. 2
    洗涤washed with water twice
  3. 3
    干燥The organic layer was dried over magnesium sulfate
  4. 4
    其他Removal of the solvent
  5. 5
    其他gave a brownish oil, which
  6. 6
    workup.DISTILLATIONwas purified by distillation under reduced pressure

实验过程

A mixture of 2-formyl-5-methylthiophene (12.6 g, 0.1 mol), methyl orthoformate (31.8 g) and a catalytic amount of p-toluene-sulfonic acid in toluene (120 ml) was refluxed for 6 hours. To the cooled reaction mixture was added ethyl acetate and washed with water twice. The organic layer was dried over magnesium sulfate. Removal of the solvent gave a brownish oil, which was purified by distillation under reduced pressure to afford 2-dimethoxymethyl-5-methylthiophene (13.54 g, 78.5% yield) as a yellow oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05763437uspto-grants-1998_06