تفاعل #1233

ord-9664b54f4f6141978a503b896b8ef7fd

معادلة التفاعل

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

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture was heated
  2. 2
    درجة الحرارةat reflux for twelve hours
  3. 3
    أخرىthe reaction medium evaporated
  4. 4
    أخرىwater, the organic phase decanted off
  5. 5
    تجفيفdried over magnesium sulfate
  6. 6
    أخرىevaporated
  7. 7
    أخرىThe residue was triturated in methanol
  8. 8
    ترشيحfiltered
  9. 9
    أخرى21.9 g (85%) of the expected methyl ester of melting point 58°-59° C. were recovered

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05723499uspto-grants-1998_03