反应详情

To a solution of 3-amino-1,2-benzisoxazole (3.5 g) in N,N-dimethylformamide (DMF) (100 ml) was added sodium hydride (0.8 g) under nitrogen. The reaction was stirred one hour at ambient temperature. A solution of 4-(2-chloroethyl)morpholine (4.0 g) in DMF (50 ml) was added followed by heating to 120° C. for one hour. TLC (5% MeOH/DCM) analysis revealed the absence of starting material. The reaction was quenched with water and extracted with EtOAc. The organic layer was washed with water, dried (MgSO4), and concentrated in vacuo. Flash column chromatography (silica gel) eluting with 1.5-2.5% MeOH/DCM afforded the product (2.5 g), m.p. 79-80° C.

1. temperatureby heating to 120° C. for one hour
2. customThe reaction was quenched with water
3. extractionextracted with EtOAc
4. washThe organic layer was washed with water
5. dry with materialdried (MgSO4)
6. concentrationconcentrated in vacuo
7. washFlash column chromatography (silica gel) eluting with 1.5-2.5% MeOH/DCM