반응 #1233

ord-9664b54f4f6141978a503b896b8ef7fd

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture was heated
  2. 2
    온도at reflux for twelve hours
  3. 3
    기타the reaction medium evaporated
  4. 4
    기타water, the organic phase decanted off
  5. 5
    건조dried over magnesium sulfate
  6. 6
    기타evaporated
  7. 7
    기타The residue was triturated in methanol
  8. 8
    여과filtered
  9. 9
    기타21.9 g (85%) of the expected methyl ester of melting point 58°-59° C. were recovered

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05723499uspto-grants-1998_03