反応 #632029

反応方程式

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

溶媒

ethanol

反応条件

後処理

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

実験手順

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).

出典