反应详情

温度

140 °C

To a sealed tube was added 3-chloro-6-methoxy-1,2-benzisoxazole (2.0 g) and N-methylethylenediamine (4.8 g). The reaction was heated to 140° C. over 48 hours and then cooled to room temperature. The residue was partitioned between EtOAc and brine, washed with brine (4×) and the organic phase was dried over MgSO4 and concentrated in vacuo. Flash chromatography (silica gel) eluting with 5% acetone/CH2Cl2 provided a residue upon evaporation (0.4 g) m.p. 136°-137° C.

1. temperaturecooled to room temperature
2. customThe residue was partitioned between EtOAc and brine
3. washwashed with brine (4×)
4. dry with materialthe organic phase was dried over MgSO4
5. concentrationconcentrated in vacuo
6. washFlash chromatography (silica gel) eluting with 5% acetone/CH2Cl2
7. customprovided a residue
8. customupon evaporation (0.4 g) m.p. 136°-137° C.