反应详情

To sodium hydride (93.5 g, 3.9 mol) suspended in tetrahydrofuran (300 mL) was added 2,6-dimethylhept-5-en-2-ol (500 g, 3.5 mol) in tetrahydrofuran (1000 mL). The mixture was heated at reflux until gas evolution was complete. Dimethylsulfate (274 mL, 2.9 mol) in tetrahydrofuran (226 mL) was added to the cold (0° C.) mixture. After standing for 16 h, the mixture was heated at reflux for 7 hours. Aqueous workup yielded 2,6-dimethyl-2-methoxyhept-5-ene, bp40 65°-68° C. (461.5 g); NMR(CDCl3)δ1.2(s,6H), 1.4-1.6(m,2H), 1.6(s,3H), 1.7(s,3H), 1.9-2.1(m,2H), 3.2(s,3H), 5.1-5.2(m,1H); IR(neat) 2970, 2932, 1462, 1442, 1373, 1357, 1195, 1072 cm-1 ; MS(m/e) 41, 67, 73, 109, 124, 142.

1. temperatureThe mixture was heated
2. temperatureat reflux until gas evolution
3. temperaturethe mixture was heated
4. temperatureat reflux for 7 hours