Hydrogen iodide → 4-(3,5-dimethyl-1H-1,2,4-triazol-1-yl)-6-iodo-2-methylpyrimidine
反応式
Cl[C:2]1[CH:7]=[C:6]([N:8]2[C:12]([CH3:13])=[N:11][C:10]([CH3:14])=[N:9]2)[N:5]=[C:4]([CH3:15])[N:3]=1.[IH:16]>O>[CH3:14][C:10]1[N:11]=[C:12]([CH3:13])[N:8]([C:6]2[CH:7]=[C:2]([I:16])[N:3]=[C:4]([CH3:15])[N:5]=2)[N:9]=1参加物
4
反応条件
- 温度
- 70 °C
実験手順
To a mixture of 4-chloro-6-(3,5-dimethyl-1H-1,2,4-triazol-1-yl)-2-methylpyrimidine (2.00 g, 8.9 mmol), KI (4.44 g, 26.8 mmol) was added 57% aq. HI solution (20 mL, 89.2 mmol). After heating at 70° C. for 5 min, water (20 mL) was added to the reaction mixture. The white solid was filtered, rinsed with water, and dried under vacuum to give Intermediate 2 as a white solid. 1H NMR (400 MHz, DMSO) δ 8.06 (s, 1H), 2.78 (s, 3H), 2.62 (s, 3H), 2.30 (s, 3H). MS: m/z=316.1 (M+H).
後処理
- filtrationThe white solid was filtered
- washrinsed with water
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-a30628f94b1d437fb34dc88bc1e37612
- 出典データセット
- uspto-grants-2016_03
- 特許番号
- US09284302B2
反応ノート
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