Ammonia → HCID 66915610、化合物
反応式
[Br:1][C:2]1[N:3]=[C:4]([I:12])[N:5]2[CH:10]=[CH:9][N:8]=[C:7](Cl)[C:6]=12.[NH3:13]>CC(O)C.O>[Br:1][C:2]1[N:3]=[C:4]([I:12])[N:5]2[CH:10]=[CH:9][N:8]=[C:7]([NH2:13])[C:6]=12参加物
5
反応条件
- 温度
- 95 °C
実験手順
To a stirred solution of 1-bromo-8-chloro-3-iodo-imidazo[1,5-a]pyrazine (250.00 mg, 0.696 mmol) in i-PrOH (8 mL) in a Parr bomb was added 7 mL ammonia in water (35%). The resulting solution was stirred at 95° C. overnight. The solvent was removed under reduced pressure and the crude material was passed through a short silica gel column (5% MeOH in DCM as eluent). The fractions were collected and combined, solvent was removed under reduced pressure to give a residue which was used in next step without further purification. MS (ES+): m/z: 338.80, 340.81 [MH+]. HPLC: tR=1.64 min (OpenLynx: polar—5 min).
後処理
- customThe solvent was removed under reduced pressure
- customThe fractions were collected
- customsolvent was removed under reduced pressure
- customto give a residue which
- customwas used in next step without further purification
- customHPLC: tR=1.64 min (OpenLynx: polar—5 min)
出典と根拠
- ORDレコード
- ord-4dadfc2af14741009edba2a075bf4547
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08481733B2
反応ノート
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