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

HRID 1438914ノート

反応式

HRID 1438914 の反応式
[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]

参加物

6

反応物 4

HCID 962WaterHCID 6101p-Toluenesulfonic acidHCID 8012ButanethiolHCID 70624727HCID 70624727、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-4b10890d253445b8ac7b2d134399e91f
出典データセット
uspto-grants-1977_11
特許番号
US04057559

反応ノート

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