反应 #5146

ord-65ea4057d75b4366aba54ef2265871f0

反应方程式

C=C(C)C(=O)Cl
methacryloyl chloride
OCCOCc1csc(Br)c1
2-bromo-4-2-hydroxyethoxymethylthiophene
c1ccncc1
pyridine
CC#N
acetonitrile
O
water
C=C(C)C(=O)OCC(OC)c1csc(Br)c1
2-bromo-4-thienyl-methoxyethyl methacrylate

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGAfter stirring the mixture for one hour
  2. 2
    萃取The ethyl acetate layer was extracted
  3. 3
    浓缩concentrated
  4. 4
    其他purified by column chromatography

实验过程

While stirring a mixture of 0.1 mol of 2-bromo-4-2-hydroxyethoxymethylthiophene, 0.1 mol of pyridine, and 100 ml of acetonitrile at a temperature of lower than 10° C., 0.1 mol of methacryloyl chloride was added dropwise to the mixture over a period of 30 minutes. After stirring the mixture for one hour, 200 ml of ethyl acetate and 200 ml of water were added to the mixture. The ethyl acetate layer was extracted, concentrated, and purified by column chromatography to provide 22.1 g of 2-bromo-4-thienyl-methoxyethyl methacrylate (5-A).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05243004uspto-grants-1993_09