Methyl chloroformate → 6-chloro-4-nitro-1H-pyrrolo[2,3-b]pyridine
反応式
[N+:1]([C:4]1[CH:9]=[CH:8][N+:7]([O-])=[C:6]2[NH:11][CH:12]=[CH:13][C:5]=12)([O-:3])=[O:2].C[Si](C)(C)N[Si](C)(C)C.[Cl:23]C(OC)=O>C1COCC1>[Cl:23][C:8]1[N:7]=[C:6]2[NH:11][CH:12]=[CH:13][C:5]2=[C:4]([N+:1]([O-:3])=[O:2])[CH:9]=1参加物
5
実験手順
Under an atmosphere of argon, 5.00 g (27.9 mmol) of 4-nitro-1H-pyrrolo[2,3-b]pyridine 7-oxide and 11.8 ml (55.8 mmol) of hexamethyldisilazane are initially charged in 290 ml of THF. At RT, 10.8 ml (140 mmol) of methyl chloroformate are added. The solution is stirred at RT overnight. The reaction solution is filtered through a silica gel cartridge, and the cartridge is washed with dichloromethane/methanol 10:1.
後処理
- filtrationThe reaction solution is filtered through a silica gel cartridge
- washthe cartridge is washed with dichloromethane/methanol 10:1
出典と根拠
- ORDレコード
- ord-c437acc50e064b809657cfdfa9de6046
- 出典データセット
- uspto-grants-2012_12
- 特許番号
- US08329716B2
反応ノート
読み込み中…