反应详情

温度

75 °C

N-(2-{[3-chloro-1-(phenylsulfonyl)-1H-indol-5-yl]oxy}ethyl)acetamide (Intermediate 39, 1.07 g, 2.73 mmol, ca 80% pure) in EtOH (25 ml) and 2 M NaOH (5 ml) were mixed and heated at 75° C. for 1 hour. The reaction mixture was cooled, diluted with water and extracted with DCM. The organic phase was dried (MgSO4) and evaporated to give the crude material (0.287 g) as a colorless oil. The crude material (0.250 g, 0979 mmol) was dissolved in MeCN (20 ml) and POCl3 was added. The reaction mixture was heated at 120° C. for 15 minutes in a microwave heater and evaporated. The crude material was purified by preparative HPLC (XTerra C18, 50 mM NH4HCO3 pH 10-CH3CN) to give the title compound (99.7 mg) as a white solid. MS m/z 235 [M+H]+.

1. temperatureThe reaction mixture was cooled
2. extractionextracted with DCM
3. dry with materialThe organic phase was dried (MgSO4)
4. customevaporated
5. customto give the crude material (0.287 g) as a colorless oil
6. temperatureThe reaction mixture was heated at 120° C. for 15 minutes in a microwave heater
7. customevaporated
8. customThe crude material was purified by preparative HPLC (XTerra C18, 50 mM NH4HCO3 pH 10-CH3CN)