Methanol → Methyl hexyl cyclopentanone carboxylate

HRID 1076038노트

반응식

HRID 1076038 반응식
[CH2:1]([CH:7]1[CH:11]([C:12]#N)[CH2:10][CH2:9][C:8]1=[O:14])[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].[OH2:15].C1(C)C=CC(S(O)(=O)=O)=CC=1.[CH3:27][OH:28]>>[CH2:1]([CH:7]1[C:8](=[O:14])[CH2:9][CH2:10][CH:11]1[C:12]([O:28][CH3:27])=[O:15])[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6]

참가 물질

4

반응물 3

HCID 887Methanol2회HCID 521998p-Toluenesulfonic acid monohydrateHCID 112984832-n-Hexyl-3-cyanocyclopentanone2회

생성물 1

HCID 162249Methyl hexyl cyclopentanone carboxylate

실험 절차

In a 100 ml round bottomed flask fitted with a mechanical stirrer and a reflux condenser, are placed 19.3 g 2-n-hexyl-3-cyanocyclopentanone, 3.2 g of methanol and 19 g of 2-n-hexyl-3-cyanocyclopentanone, 3.2 g of methanol and 19 g of p-toluene-sulfonic acid monohydrate. The reaction mixture is stirred at reflux temperature for 6 hours. The reaction mixture is then cooled to room temperature and poured into 200 ml of ice cold water. The organic layer is separated and the water phase is extracted with pentane. The combined organic layer and pentane extract are washed with sodium carbonate solution and water and dried over anhydrous sodium sulphate. The solvent is distilled off at atmospheric pressure and the residue is distilled through a short Vigreux column.

후처리

  1. customIn a 100 ml round bottomed flask fitted with a mechanical stirrer and a reflux condenser
  2. temperatureat reflux temperature for 6 hours
  3. customThe organic layer is separated
  4. extractionthe water phase is extracted with pentane
  5. extractionThe combined organic layer and pentane extract
  6. washare washed with sodium carbonate solution and water
  7. dry with materialdried over anhydrous sodium sulphate
  8. distillationThe solvent is distilled off at atmospheric pressure
  9. distillationthe residue is distilled through a short Vigreux column

출처 및 근거

ORD 기록
ord-6ef6cf12622441aa9882e50ff01d12ef
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03954834

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