反应 #1269871

反应方程式

5-chloro-1-phenyl tetrazole

potassium carbonate

2,6-diazaspiro[3.3]heptane

→

2-(1-phenyl-1H-tetrazol-5-yl)-2,6-diazaspiro[3.3]heptane

收率 37.3%

溶剂

ethanol

ethanol

反应条件

后处理

1. 1
   workup.STIRRINGto stir for 5 hours at room temperature
2. 2
   其他The reaction mixture was evaporated
3. 3
   其他to give a residue which
4. 4
   其他was partitioned between water (10 mL) and EtOAc (20 mL)
5. 5
   萃取The aqueous layer was extracted with ethyl acetate (3×20 mL)
6. 6
   干燥The combined organic layer was dried over anhydrous Na2SO4
7. 7
   浓缩concentrated under reduced pressure
8. 8
   其他gave crude product which
9. 9
   其他was purified by column chromatography

实验过程

To potassium carbonate (76 mg) taken in ethanol (2.0 mL), a solution of 2,6-diazaspiro[3.3]heptane (220 mg in 2.0 ml of ethanol) was added at room temperature. The reaction mixture was stirred for 30 minutes at room temperature and a solution of 5-chloro-1-phenyl tetrazole (0.1 g) in ethanol (2.0 mL) was added very slowly. The reaction mixture was allowed to stir for 5 hours at room temperature. The reaction mixture was evaporated to give a residue which was partitioned between water (10 mL) and EtOAc (20 mL). The aqueous layer was extracted with ethyl acetate (3×20 mL). The combined organic layer was dried over anhydrous Na2SO4 and concentrated under reduced pressure gave crude product which was purified by column chromatography using methanol\dichloromethane (1:9) as eluent to afford 2-(1-phenyl-1H-tetrazol-5-yl)-2,6-diazaspiro[3.3]heptane (50 mg).

来源