Actually, I love my glass as much as the product! 1g KOH was added to 53g Allylbenzene and heated to 120°C with stiring and water left to evaporate for about 10 minutes. The KOH turned brown and I couldn't see any water coming off, but the allyl evaporates quickly.
Added condenser, thermometer, took oil bath to 170°C, vapor temp was 158°C and refluxed for 23hrs. No temp rise. Why? This is simple isn't it! I've made safrole via grignard, Why can't I do this?
Anyway, 25ml Butanol was added and everything set up for fractional distillation to see how much water was still in the system. Oil was bath at 150°C when the azeotrope came over at 93°C, but it was very small. One drop of water, that's it. Is that enough to prevent isomerisation?
Regards,
FF.