Methanol → Methyl 4-Iodo-3-methylbenzoate

HRID 1137

반응식

HRID 1137 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[I:11])[C:5]([OH:7])=[O:6].S(=O)(=O)(O)O.[CH3:17]O>>[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[I:11])[C:5]([O:7][CH3:17])=[O:6]

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 15173224-Iodo-3-methylbenzoic acid

생성물 1

HCID 231757Methyl 4-Iodo-3-methylbenzoate

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.

후처리

  1. temperatureThe mixture was heated
  2. temperatureat reflux for twelve hours
  3. customthe reaction medium evaporated
  4. customwater, the organic phase decanted off
  5. dry with materialdried over magnesium sulfate
  6. customevaporated
  7. customThe residue was triturated in methanol
  8. filtrationfiltered
  9. custom21.9 g (85%) of the expected methyl ester of melting point 58°-59° C. were recovered

출처 및 근거

ORD 기록
ord-9664b54f4f6141978a503b896b8ef7fd
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05723499

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