Triethylsilane → HCID 13285353、化合物
反応式
[Cl:1][CH2:2][C:3]([C:5]1[C:13]2[C:8](=[N:9][CH:10]=[CH:11][CH:12]=2)[NH:7][CH:6]=1)=O.C([SiH](CC)CC)C>C(O)(C(F)(F)F)=O.CCOC(C)=O.C(=O)([O-])[O-].[Na+].[Na+]>[Cl:1][CH2:2][CH2:3][C:5]1[C:13]2[C:8](=[N:9][CH:10]=[CH:11][CH:12]=2)[NH:7][CH:6]=1参加物
6
実験手順
A stirred solution of 2-chloro-1-(1H-pyrrolo[2,3-b]pyridin-3-yl)ethanone (12.5 g) in TFA at room temperature is treated with triethylsilane (72 mL, 7 eq.), stirred for 16 h, diluted with EtOAc and saturated sodium carbonate to pH 8. The phases are separated and the organic phase is dried over MgSO4 and concentrated in vacuo. The resultant residue is purified by flash chromatography (silica gel, 10% EtOAc in ether as eluent) to give the title pyrrolo[2,3-b]pyridine compound, identified by NMR and mass spectral analyses.
後処理
- customThe phases are separated
- dry with materialthe organic phase is dried over MgSO4
- concentrationconcentrated in vacuo
- customThe resultant residue is purified by flash chromatography (silica gel, 10% EtOAc in ether as eluent)
出典と根拠
- ORDレコード
- ord-e7eded962bbd4a0bb25952179cbb735c
- 出典データセット
- uspto-grants-2007_11
- 特許番号
- US07297705B2
反応ノート
読み込み中…