反応 #92359

反応方程式

4-iodo-1H-pyrazole

K2CO3

bromocyclopentane

→

1-Cyclopentyl-4-iodo-1H-pyrazole

収率 89.5%

溶媒

DMF

反応条件

後処理

1. 1
   その他The mixture was quenched
2. 2
   抽出extracted as in Intermediate Example 5(a)
3. 3
   workup.DISTILLATIONThe solvent was distilled off
4. 4
   その他to give the product in 89.5% yield
5. 5
   その他263 [M+H]+ (rt: 1.57 min)

実験手順

To a solution of 4-iodo-1H-pyrazole (5 g, 25.78 mmol, 1.0 eq.) in DMF (25 ml) were added K2CO3 (8.908 g, 64.45 mmol, 2.5 eq.) and bromocyclopentane (4.96 g, 33.51 mmol, 1.3 eq.). The mixture was stirred at RT for 12 h. The mixture was quenched and extracted as in Intermediate Example 5(a). The solvent was distilled off to give the product in 89.5% yield. 1H NMR (300 MHz, CDCl3): δ 7.49 (s, 1H), 7.45 (s, 1H), 4.66-4.62 (m, 1H), 2.17-2.02 (m, 1H), 2.00-1.96 (m, 2H), 1.93-1.78 (m, 2H), 1.73-1.67 (m, 2H). LC-MS (ESI): Calculated mass: 262; Observed mass: 263 [M+H]+ (rt: 1.57 min).

出典