N-Iodosuccinimide → ethyl 4-iodo-5-methyl-1H-pyrazole-3-carboxylate
反応式
[CH3:1][C:2]1[CH:6]=[C:5]([C:7]([O:9][CH2:10][CH3:11])=[O:8])[NH:4][N:3]=1.C1C(=O)N([I:19])C(=O)C1>CN(C=O)C>[I:19][C:6]1[C:5]([C:7]([O:9][CH2:10][CH3:11])=[O:8])=[N:4][NH:3][C:2]=1[CH3:1]参加物
4
実験手順
To a stirred solution of ethyl 3-methylpyrazole-5-carboxylate (3.11 g, 20.17 mmol) in DMF (50 mL) under Ar at 0° C. was added NIS (5.90 g, 26.2 mmol). The reaction mixture was stirred 20 hr at rt and quenched with 500 mL of water. The resulting precipitate was collected to afford the title product (5.61 g, 20.03 mmol, 99% yield) as a white solid. tR: 3.75 min (HPLC 1); tR: 0.78 min (LC-MS 2); ESI-MS: 281 [M+H]+ (LC-MS 2)
後処理
- customquenched with 500 mL of water
- customThe resulting precipitate was collected
出典と根拠
- ORDレコード
- ord-f10b5e2764a14411aa8d29ad518682e2
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08975417B2
反応ノート
読み込み中…