Water → 2-[(Butylthio)methylene]-6-ethylcyclohexanone

HRID 1438914노트

반응식

HRID 1438914 반응식
[CH2:1]([CH:3]1[CH2:8][CH2:7][CH2:6][C:5](=[CH:9]O)[C:4]1=[O:11])[CH3:2].[CH2:12]([SH:16])[CH2:13][CH2:14][CH3:15].C1(C)C=CC(S(O)(=O)=O)=CC=1.O>C1C=CC=CC=1>[CH2:12]([S:16][CH:9]=[C:5]1[CH2:6][CH2:7][CH2:8][CH:3]([CH2:1][CH3:2])[C:4]1=[O:11])[CH2:13][CH2:14][CH3:15]

참가 물질

6

반응물 4

HCID 962WaterHCID 6101p-Toluenesulfonic acidHCID 8012ButanethiolHCID 70624727HCID 70624727, 화합물

생성물 1

HCID 537663082-[(Butylthio)methylene]-6-ethylcyclohexanone

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A solution of 2-ethyl-6-(hydroxymethylene)cyclohexanone (43.0 g, 0.277 mole), described in Example 2, butylmercaptan (28.6 g, 0.318 mole) and p-toluenesulfonic acid (50 mg) in dry benzene (200 ml) is heated at reflux under nitrogen for 4 hr using a Dean-Stark water separator. The reaction mixture is cooled and washed with saturated aqueous sodium bicarbonate (50 ml), water and brine, then dried (MgSO4). After removal of the solvent at reduced pressure the residue is distilled to give the title compound, bp 110° - 115° C/1.5 mm, nmr (CDCl3) δ 0.92 (6H), 7.5 (m,1H).

후처리

  1. temperatureis heated
  2. temperatureat reflux under nitrogen for 4 hr
  3. temperatureThe reaction mixture is cooled
  4. washwashed with saturated aqueous sodium bicarbonate (50 ml), water and brine
  5. dry with materialdried (MgSO4)
  6. customAfter removal of the solvent at reduced pressure the residue
  7. distillationis distilled

출처 및 근거

ORD 기록
ord-4b10890d253445b8ac7b2d134399e91f
출처 데이터셋
uspto-grants-1977_11
특허 번호
US04057559

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