تفاعل #1318
ord-6724f220dc7c4e89ac64b79ac6a33d74
معادلة التفاعل
4-iodobenzoic acid
ethanol
thionyl chloride
→
title compound
Ethyl-4-iodobenzoate
الكواشف
لا شيء
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةthe mixture was then heated
- 2درجة الحرارةat reflux for 3 hours
- 3أخرىSolvent was removed in vacuo
- 4workup.DISSOLUTIONthe residue was dissolved in 100 ml ether
- 5غسيلThe ether solution was washed with saturated NaHCO3 and saturated NaCl solutions
- 6تجفيفdried (MgSO4)
- 7أخرىSolvent was then removed in vacuo
- 8workup.DISTILLATIONthe residue kugelrohr distilled (100 degrees C.; 0.55 mm)
الإجراء التجريبي
To a suspension of 10 g (40.32 mmol) of 4-iodobenzoic acid in 100 ml absolute ethanol was added 2 ml thionyl chloride and the mixture was then heated at reflux for 3 hours. Solvent was removed in vacuo and the residue was dissolved in 100 ml ether. The ether solution was washed with saturated NaHCO3 and saturated NaCl solutions and dried (MgSO4). Solvent was then removed in vacuo and the residue kugelrohr distilled (100 degrees C.; 0.55 mm) to give the title compound as a colorless oil, PMR (CDCl3): δ1.42 (3H, t, J~7 Hz), 4.4 (2H, q, J~7 Hz), 7.8 (4H).