Bromocyclopentane → 1-cyclopentyl-4-iodo-1H-pyrazole
반응식
[I:1][C:2]1[CH:3]=[N:4][NH:5][CH:6]=1.C([O-])([O-])=O.[K+].[K+].Br[CH:14]1[CH2:18][CH2:17][CH2:16][CH2:15]1>CN(C=O)C>[CH:14]1([N:4]2[CH:3]=[C:2]([I:1])[CH:6]=[N:5]2)[CH2:18][CH2:17][CH2:16][CH2:15]1참가 물질
5
실험 절차
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).
후처리
- customThe mixture was quenched
- extractionextracted as in Intermediate Example 5(a)
- distillationThe solvent was distilled off
- customto give the product in 89.5% yield
- custom263 [M+H]+ (rt: 1.57 min)
출처 및 근거
- ORD 기록
- ord-58880dbf79124678b073a50a8366605f
- 출처 데이터셋
- uspto-grants-2016_09
- 특허 번호
- US09447091B2
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