反应详情

Diethyl 2-ethoxycarbonyl-2-n-propyl-succinate (55.8 g) in dry ether (50 ml.) was added slowly to a stirred suspension of lithium aluminium hydride (14.7 g.) in dry ether (150 ml.) at 0°, under a current of nitrogen. The mixture was stirred at room temperature for three hours and then refluxed, with stirring for four hours. A solution of potassium hydroxide (30.0 g.), potassium dihydrogen phosphate (22.0 g.) and potassium monohydrogen phosphate (22.0 g.) in water (200 ml.) was added to the cooled reaction mixture. The pH was adjusted to 5.0 with glacial acetic acid. The solid was removed by filtration and washed with water (40 ml.) The combined filtrates and washings were evaporated in vacuo. The residue was washed with acetone (3×100 ml). The acetone washings were evaporated in vacuo. The residue was washed with chloroform (3×100 ml.) and the washings were evaporated in vacuo, Toluene was added and the residue was evaporated in vacuo. 3,3-Di-(hydroxymethyl)-hexan-1-ol was obtained as a colourless oil and was used without further purification.

1. temperaturerefluxed
2. stirringwith stirring for four hours
3. customThe solid was removed by filtration
4. washwashed with water (40 ml.) The combined filtrates and washings
5. customwere evaporated in vacuo
6. washThe residue was washed with acetone (3×100 ml)
7. customThe acetone washings were evaporated in vacuo
8. washThe residue was washed with chloroform (3×100 ml.)
9. customthe washings were evaporated in vacuo, Toluene
10. additionwas added
11. customthe residue was evaporated in vacuo