反应 #1946546

ord-158dae43966a4dd5b0fc23a9a3e6ced4

反应方程式

O
water
C=C(C)C(=O)Nc1ccc(C(=O)O)c(O)c1
4-methacrylamidosalicylic acid
CC(=O)OC(C)=O
acetic anhydride
C=C(C)C(=O)Nc1ccc(C(=O)OC(C)=O)c(O)c1
O-acetyl-4-methacrylamidosalicylic acid

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.WAITfor an additional 6 hours at room temperature
  2. 2
    workup.ADDITIONThe reaction mixture is then poured into 800 g
  3. 3
    其他The solid product precipitates from solution
  4. 4
    过滤is collected by filtration
  5. 5
    其他air dried at room temperature
  6. 6
    其他to afford A-4-MASA in quantitative yield

实验过程

A few drops of concentrated sulfuric acid is added to a stirring solution of 35.0 g of 4-methacrylamidosalicylic acid (prepared according to Example 1) in 350 mL of acetic anhydride at 0° C. The solution is stirred for 60 minutes at 0° C. and then for an additional 6 hours at room temperature. The reaction mixture is then poured into 800 g of cold deionized water. The solid product precipitates from solution, and is collected by filtration. The product is then air dried at room temperature to afford A-4-MASA in quantitative yield.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06527959B1uspto-grants-2003_03