反応 #674310

反応方程式

4-iodo-1H-pyrazole

tert-butyl 7-(methylsulfonyloxy)-2-azaspiro[3.5]nonane-2-carboxylate

4-iodo-1H-pyrazole

Cs2CO3

→

tert-butyl 7-(4-iodo-1H-pyrazol-1-yl)-2-azaspiro[3.5]nonane-2-carboxylate

収率 81.0%

溶媒

DMF

反応条件

後処理

1. 1
   濃縮It was concentrated by rotary evaporator in vacuo
2. 2
   その他to give the residue which
3. 3
   その他was purified by CombiFlash (12 g silica gel column, EtOAc/Hex: 0-40%)

実験手順

To a solution of 4-iodo-1H-pyrazole and tert-butyl 7-(methylsulfonyloxy)-2-azaspiro[3.5]nonane-2-carboxylate (70 mg, 0.219 mmol, 1.0 equiv) and 4-iodo-1H-pyrazole in DMF (1 mL) was added Cs2CO3 (79 mg, 0.241 mmol, 1.1 equiv). The mixture was stirred at 80° C. for 3 hrs. It was concentrated by rotary evaporator in vacuo to give the residue which was purified by CombiFlash (12 g silica gel column, EtOAc/Hex: 0-40%) to afford 74 mg (yield 81%) of tert-butyl 7-(4-iodo-1H-pyrazol-1-yl)-2-azaspiro[3.5]nonane-2-carboxylate as a off-white solid.

出典