反应 #1233

ord-9664b54f4f6141978a503b896b8ef7fd

反应方程式

Cc1cc(C(=O)O)ccc1I
3-methyl-4-iodobenzoic acid
CO
methanol
O=S(=O)(O)O
sulfuric acid
COC(=O)c1ccc(I)c(C)c1
methyl 3-methyl-4-iodobenzoate

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The mixture was heated
  2. 2
    温度at reflux for twelve hours
  3. 3
    其他the reaction medium evaporated
  4. 4
    其他water, the organic phase decanted off
  5. 5
    干燥dried over magnesium sulfate
  6. 6
    其他evaporated
  7. 7
    其他The residue was triturated in methanol
  8. 8
    过滤filtered
  9. 9
    其他21.9 g (85%) of the expected methyl ester of melting point 58°-59° C. were recovered

实验过程

24.4 g (0.093 mol) of 3-methyl-4-iodobenzoic acid and 250 ml of methanol were introduced into a round-bottomed flask and 2.5 ml of concentrated sulfuric acid were added dropwise. The mixture was heated at reflux for twelve hours, the reaction medium evaporated, taken up in ethyl acetate and water, the organic phase decanted off, dried over magnesium sulfate and evaporated. The residue was triturated in methanol and filtered; 21.9 g (85%) of the expected methyl ester of melting point 58°-59° C. were recovered.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05723499uspto-grants-1998_03