反应详情

温度

100 °C

In a 5 ml microwave reaction vessel was added 6-(5-{3-chloro-4-[(1-methylethyl)oxy]phenyl}-1,2,4-oxadiazol-3-yl)-2,3,4,5-tetrahydro-1H-3-benzazepine hydrochloride (Example 8) (110 mg, 0.262 mmol). Then potassium carbonate (101 mg) was added followed by 1,1-dimethylethyl bromoacetate (51.0 mg, 0.262 mmol). The reaction mixture was heated at 100° C. for 10 minutes. The cooled reaction mixture was diluted with DCM (5 ml) and purified by SCX (washing with methanol and eluting the crude amino ester with methanolic ammonia). 1,1-dimethylethyl [6-(5-{3-chloro-4-[(1-methylethyl)oxy]phenyl}-1,2,4-oxadiazol-3-yl)-1,2,4,5-tetrahydro-3H-3-benzazepin-3-yl]acetate (120 mg, 0.241 mmol, 92% yield) was isolated as a pale yellow oil. MS (ES) C27H3235ClN3O4 requires 497; found 498 [M+H]+.

1. customThe cooled reaction mixture
2. custompurified by SCX (
3. washwashing with methanol
4. washeluting the crude amino ester with methanolic ammonia)