反应详情

温度

45 °C

CDI (63.2 mg, 0.39 mmol) is added to a solution of 2-(4,5,6,7-tetrahydro-1-phenyl-1H-indazol-4-yl)acetic acid (100 mg, 0.39 mmol) in CH2Cl2 (20 mL) cooled in an ice bath, and is heated to 45° C. for 2.5 hours. Then it is cooled to 0° C. and azacycloheptane (38.7 mg, 0.39 mmol) is added and is heated at 45° C. for 1 hour. The solvent is evaporated under reduced pressure, diluted in AcOEt and washed with diluted HCl. The organic phase is dried and evaporated under reduced pressure. The resulting crude product is purified by means of silica gel chromatography, giving 1-(2-(4,5,6,7-tetrahydro-1-phenyl-1H-indazol-4-yl)acetyl)azepane (45 mg, 0.13 mmol, 33%, oil).

1. temperaturecooled in an ice bath
2. temperatureThen it is cooled to 0° C.
3. temperatureis heated at 45° C. for 1 hour
4. customThe solvent is evaporated under reduced pressure
5. additiondiluted in AcOEt
6. washwashed with diluted HCl
7. customThe organic phase is dried
8. customevaporated under reduced pressure
9. customThe resulting crude product is purified by means of silica gel chromatography