反应详情

温度

150 °C

2.3 g. Sodium are dissolved by warming in 44 ml. butane-1,4-diol, 38 ml. 1-bromotridecane are added thereto and the reaction mixture is stirred for 5 hours at a bath temperature of 150° C. After cooling, extraction is carried out with a mixture of diethyl ether-ligroin (1:2 v/v), the extract is evaporated and the residue is purified on a silica gel column by elution with ligroin which is subsequently replaced by diethyl ether-ligroin (1:1 v/v). The desired fractions are collected and evaporated. 19.4 g. (71% of theory) of thin layer chromatographically uniform 4-tridecyloxybutanol are thus obtained; m.p. 26°-29° C.

1. temperatureby warming in 44 ml
2. temperatureAfter cooling
3. extractionextraction
4. additionis carried out with a mixture of diethyl ether-ligroin (1:2 v/v)
5. customthe extract is evaporated
6. customthe residue is purified on a silica gel column by elution with ligroin which
7. customThe desired fractions are collected
8. customevaporated