Potassium Carbonate → HCID 21894750、化合物
反応式
C([O-])([O-])=O.[K+].[K+].[Br:7][C:8]1[CH:9]=[C:10]2[C:14](=[CH:15][CH:16]=1)[NH:13][N:12]=[CH:11]2>CN(C=O)C>[Br:7][C:8]1[CH:9]=[C:10]2[C:14](=[CH:15][CH:16]=1)[N:13]([CH2:9][CH:10]([CH3:14])[CH3:11])[N:12]=[CH:11]2参加物
4
反応条件
- 温度
- 105 °C
実験手順
K2CO3 was added to a solution of 5-bromoindazole and in DMF. The mixture was heated to 105° C. After disappearance of 5-bromoindazole the reaction mixture was poured onto DCM/brine. The two layers were separated and the aqueous layer was extracted with DCM (2×) and checked by TLC. The combined organics were washed with H2O (2×) and brine and dried over Na2SO4. After filtration, the filtrate was concentrated and the resulting residue was purified by chromatography with 9.5:0.5 hexane/EtOAc to provide desired product (14p).
後処理
- customThe two layers were separated
- extractionthe aqueous layer was extracted with DCM (2×)
- washThe combined organics were washed with H2O (2×) and brine
- dry with materialdried over Na2SO4
- filtrationAfter filtration
- concentrationthe filtrate was concentrated
- customthe resulting residue was purified by chromatography with 9.5:0.5 hexane/EtOAc
出典と根拠
- ORDレコード
- ord-a024798dfc2a43fd9f609bd0e287f79c
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08017641B2
反応ノート
読み込み中…