反应详情

温度

140 °C

To a sealed tube was added 3-chloro-6-methoxy-1,2-benzisoxazole (6.0 g) and N-methyl-N-[2-(4-morpholinyl)ethyl]-amine (13.8 g). The reaction was heated to 140° C. over 48 hours and then cooled to room temperature. The residue was partitioned between ethyl acetate (EtOAc) and water, extracted again with EtOAc, and the organic phase was dried over magnesium sulfate (MgSO4) and concentration in vacuo. Flash column chromatography (silica gel) eluting with 1% methanol/dichloromethane (MeOH/DCM) provided the product (4.7 g), m.p. 43-44° C.

1. temperaturecooled to room temperature
2. customThe residue was partitioned between ethyl acetate (EtOAc) and water
3. extractionextracted again with EtOAc
4. dry with materialthe organic phase was dried over magnesium sulfate (MgSO4) and concentration in vacuo
5. washFlash column chromatography (silica gel) eluting with 1% methanol/dichloromethane (MeOH/DCM)