反应 #632029

反应方程式

hydrazine

6-Chloro-1,4-ethano-8-phenyl-1,2,3,4-tetrahydro-1,5-naphthyridine

hydrazine

HCl

→

6-hydrazino-1,4-ethano-8-phenyl-1,2,3,4-tetrahydro-1,5-naphthyridine

溶剂

ethanol

反应条件

后处理

1. 1
   温度The reaction mixture was then heated in a screw
2. 2
   其他cap pressure tube at 150° C. until LCMS
3. 3
   浓缩concentrated under vacuum
4. 4
   其他The residue was partitioned between chloroform and brine
5. 5
   干燥The organic layer was dried over anhydrous sodium sulfate
6. 6
   浓缩concentrated under vacuum

实验过程

6-Chloro-1,4-ethano-8-phenyl-1,2,3,4-tetrahydro-1,5-naphthyridine (1.03 g) was treated with anhydrous ethanol (10 mL), anhydrous hydrazine (Aldrich, 4.0 mL) and concentrated HCl (0.4 mL). The reaction mixture was then heated in a screw cap pressure tube at 150° C. until LCMS showed complete conversion to the hydrazine (approx. 96 h). The reaction mixture was cooled to ambient temperature, then concentrated under vacuum. The residue was partitioned between chloroform and brine. The organic layer was dried over anhydrous sodium sulfate and concentrated under vacuum to give 6-hydrazino-1,4-ethano-8-phenyl-1,2,3,4-tetrahydro-1,5-naphthyridine as a pale yellow solid (0.68 g).

来源