Реакция #1233

ord-9664b54f4f6141978a503b896b8ef7fd

Уравнение реакции

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

Реагенты

Нет

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe mixture was heated
  2. 2
    Температураat reflux for twelve hours
  3. 3
    Другоеthe reaction medium evaporated
  4. 4
    Другоеwater, the organic phase decanted off
  5. 5
    Сушкаdried over magnesium sulfate
  6. 6
    Другоеevaporated
  7. 7
    ДругоеThe residue was triturated in methanol
  8. 8
    Фильтрацияfiltered
  9. 9
    Другое21.9 g (85%) of the expected methyl ester of melting point 58°-59° C. were recovered

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05723499uspto-grants-1998_03