Ethyl bromoacetate → Ethyl 1H-1,2,4-triazole-1-acetate
反応式
[NH:1]1[CH:5]=[N:4][CH:3]=[N:2]1.C([O-])([O-])=O.[K+].[K+].Br[CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15]>CN(C=O)C>[N:1]1([CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:5]=[N:4][CH:3]=[N:2]1参加物
5
実験手順
To a solution of 1H-1,2,4-triazol (2 g, 29.9 mmol, 1.0 eq) in DMF were added K2CO3 (12.3 g, 88.9 mmol, 3 eq.) and ethyl 2-bromoacetate (4.8 g, 29.9 mmol, 1 eq). The mixture was stirred at RT for 16 h. The mixture was quenched and extracted as in Intermediate Example 5(a). The solvent was distilled off to give the product in 65% yield (3 g). LC-MS (ESI): Calculated mass: 155.0; Observed mass: 156.1 [M+H]+ (rt: 0.113 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 65% yield (3 g)
- custom156.1 [M+H]+ (rt: 0.113 min)
出典と根拠
- ORDレコード
- ord-509fe4691649464e92776e45b5ffda9f
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09447091B2
反応ノート
読み込み中…