Bromocyclopentane → 1-cyclopentyl-4-iodo-1H-pyrazole
反応式
[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]1参加物
5
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).
後処理
- 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)
出典と根拠
- ORDレコード
- ord-58880dbf79124678b073a50a8366605f
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09447091B2
反応ノート
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