6-(methylsulfanyl)-1H-indole-2-carboxylic acid → 6-(Methylsulfanyl)-1H-indole
反応式
[CH3:1][S:2][C:3]1[CH:11]=[C:10]2[C:6]([CH:7]=[C:8](C(O)=O)[NH:9]2)=[CH:5][CH:4]=1>N1C2C(=CC=CC=2)C=CC=1>[CH3:1][S:2][C:3]1[CH:11]=[C:10]2[C:6]([CH:7]=[CH:8][NH:9]2)=[CH:5][CH:4]=1参加物
3
反応条件
- 温度
- 215 °C
実験手順
A mixture of 6-methylsulfanyl-1H-indole-2-carboxylic acid (9.6 g, 46 mmol), Cu powder (2.1 g, 33 mmol) and quinoline (100 ml) was heated at 215° C. for 3 hours. The mixture was cooled to room temperature, filtered through celite, and the filtrate diluted with H2O (500 mL). The cooled mixture was acidified with concentrated HCl (pH=1), and extracted with EtOAc. The organic fraction was washed with saturated NaCl solution, dried over MgSO4, filtered and evaporated to give of 6-Methylsulfanyl-1H-indole (6.8 g, 90%) after purification by flash column chromatography.
後処理
- temperatureThe mixture was cooled to room temperature
- filtrationfiltered through celite
- additionthe filtrate diluted with H2O (500 mL)
- extractionextracted with EtOAc
- washThe organic fraction was washed with saturated NaCl solution
- dry with materialdried over MgSO4
- filtrationfiltered
- customevaporated
出典と根拠
- ORDレコード
- ord-1e46f9022ba945e697bdd1f5b670b94d
- 出典データセット
- uspto-grants-1999_04
- 特許番号
- US05891901
反応ノート
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