反应详情

A mixture of intermediates 1 (1.0 g, 5.71 mmol) and 2 (2.07 g, 6.86 mmol) in 4% sulphuric acid (30 ml) was heated at reflux for 48 h. The solution was cooled in an ice-bath, basified with solid K2CO3 and extracted with butan-1-ol (×3). The solvent was removed under vacuum and azeotroped with hexane (×2). The crude product was chromatographed through silica gel eluting with CH2Cl2 /MeOH/NH3 (30:8:1) to give the title-indole (282 mg, 17%). The succinate hemihydrate salt was prepared: mp 227°-228° C. (Found: C, 59.11; H, 6.58; N, 22.54.

1. temperaturewas heated
2. temperatureat reflux for 48 h
3. temperatureThe solution was cooled in an ice-bath
4. extractionextracted with butan-1-ol (×3)
5. customThe solvent was removed under vacuum
6. customazeotroped with hexane (×2)
7. customThe crude product was chromatographed through silica gel eluting with CH2Cl2 /MeOH/NH3 (30:8:1)