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 (from example XVI) and 11.8 ml (55.8 mmol) of hexamethyldisilazane are initially charged in 290 ml of THF. At room temperature, 10.8 ml (139.6 mmol) of methyl chloroformate are added. The solution is stirred at RT overnight. The reaction solution is filtered through a silica gel cartridge, and is then washed with DCM/methanol 10:1.
後処理
- filtrationThe reaction solution is filtered through a silica gel cartridge
- washis then washed with DCM/methanol 10:1
出典と根拠
- ORDレコード
- ord-cd4d09d395a04def8707814160ffa2fb
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07737153B2
反応ノート
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