反应详情

温度

30 °C

A mixture of 15.2 g (0.045 mole) of 1-(5-methyl-1,3-dioxan-5-yl)-2-(1,2,4-triazol-1-yl)-3-(4-chlorophenyl)-propan-1-ol, 100 g of 1-chloropropane, 3 g of tetrabutylammonium bisulfate and 65 g of 50% strength sodium hydroxide solution is heated for 36 hours at 30° C., with vigorous stirring. 300 ml of water are then added and the batch is extracted with twice 150 ml of methylene chloride. The combined extracts are extracted by shaking with eight time 100 ml of water, dried over magnesium sulfate and evaporated down. The residue crystallizes after addition of 20 ml of petroleum ether and 5 ml of ether. 12 g (70.3%) of 1-(5-methyl-1,3-dioxan-5-yl)-1-n-propoxy-2-(1,2,4-triazol-1-yl)-3-(4-chlorophenyl)-propane are obtained as white crystals of melting point 94°-96° C.

1. extractionthe batch is extracted with twice 150 ml of methylene chloride
2. extractionThe combined extracts are extracted
3. dry with materialdried over magnesium sulfate
4. customevaporated down
5. customThe residue crystallizes
6. additionafter addition of 20 ml of petroleum ether and 5 ml of ether