反应详情

3.2 g 1,6-dimethyl-8β-azidomethyl-9, 10-didehydroergoline in 150 mls of isopropyl alcohol are treated with 6.4 g NaBH4 and heated to reflux under stirring and under nitrogen atmosphere for 24 hours. After this time further 2 g of NaBH4 are added and the heating is continued for 24 hours more. The reaction mixture is poured into water and extracted with chloroform. The chloroform extract is chromatographed onto SiO2 and the product is eluted with CH2Cl2 /MeOH/NH4OH (9/1/0.5). 1.6 g of 1,6-dimethyl-8β-aminomethyl-9, 10-didehydroergoline are thus obtained.

1. temperatureheated
2. temperatureto reflux
3. waitthe heating is continued for 24 hours
4. extractionextracted with chloroform
5. extractionThe chloroform extract
6. customis chromatographed onto SiO2
7. washthe product is eluted with CH2Cl2 /MeOH/NH4OH (9/1/0.5)