反应详情

温度

5 °C

A solution of 0.41 g of 2-chloro-4-(o-chlorophenyl)-6H-thieno[3,2-f]-s-triazolo[4,3-a][1,4]diazepine-9-carboxylic acid ethyl ester in 6.5 ml of absolute tetrahydrofuran is added dropwise with ice-cooling and stirring to a suspension of (0.078 g) of lithium aluminium hydride in 5 ml of absolute tetrahydrofuran. After stirring for 1 hour at 5° C., there is added dropwise 0.8 ml of 0.5-N sodium hydroxide. After filtration of the solid material, the solvent is evaporated and the residue taken up in methylene chloride. The solution is washed with 0.5-N sodium hydroxide, subsequently with water and, after drying, evaporated to dryness. By crystallization of the residue from ethyl acetate, there is obtained 2-chloro-4-(o-chlorophenyl)-6H-thieno[3,2-f]-s-triazolo[4,3-a][1,4]diazepine-9-methanol, melting point 219°-221° C.

1. temperaturecooling
2. filtrationAfter filtration of the solid material
3. customthe solvent is evaporated
4. washThe solution is washed with 0.5-N sodium hydroxide, subsequently with water
5. customafter drying
6. customevaporated to dryness
7. customBy crystallization of the residue from ethyl acetate