反应详情

温度

87.5 °C

At 20-27° C., a solution of 6-ethynylspiro[4.5]decan-6-ol (180 g, 1 mol) in pyridine (1 l) was treated dropwise with POCl3 (207 g, 2 mol). The resulting mixture was heated for 5.5 h heating at 85-90° C., poured into ice and extracted twice with pentane (800 and 300 ml). The combined organic phases were washed twice with water (500 ml), with a saturated aqueous solution of NaCl (300 ml), dried (MgSO4), and concentrated. Short-path Vigreux-distillation (8 mbar, head temperature: 85° C.) of the crude product (146 g) gave 6-ethynylspiro[4.5]dec-6-ene (122.9 g, 76%).

1. temperatureThe resulting mixture was heated for 5.5 h
2. additionpoured into ice
3. extractionextracted twice with pentane (800 and 300 ml)
4. washThe combined organic phases were washed twice with water (500 ml), with a saturated aqueous solution of NaCl (300 ml)
5. dry with materialdried (MgSO4)
6. concentrationconcentrated
7. distillationShort-path Vigreux-distillation (8 mbar, head temperature: 85° C.) of the crude product (146 g)