反应详情

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).

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