反応 #1233

ord-9664b54f4f6141978a503b896b8ef7fd

反応方程式

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

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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.

出典

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