反应详情

温度

100 °C

To a slurry of 54 grams of 55% sodium hydride in 1,000 mls of toluene is portionwise added 140 grams of trans-1,2-cyclohexanediol at 90° C. with concommitant release of hydrogen. The resulting mass, containing the monosodium salt of trans-1,2-cyclohexanediol is stirred at 100° C. for 30 minutes. Ethyl bromoacetate (203 grams) is added dropwise to the stirred reaction mass at 100° C. over a 30 minute period. After stirring for 30 minutes, the mass is cooled to 20° C. Water (100 ml) is added and the organic layer is distilled to afford 130 grams of trans-hexahydro-1,4-benzodioxan-2-one. The product is purified by distillation through a 1"×12" Goodloe® packed column to afford a semi solid (m.p. 20°-22° C., bp. 97° C. at 1.2 mm).

1. customat 90° C.
2. stirringAfter stirring for 30 minutes
3. temperaturethe mass is cooled to 20° C
4. distillationthe organic layer is distilled