反应详情

To a stirred solution of 3-[[2-(4-morpholinyl)ethyl]amino]-1,2-benzisoxazol-6-ol (Example 9) (1.5 g) and 1,8-diazabicyclo[5.4.0]undec-7-ene (0.13 g) in 1,2-dichloroethane (40 ml) was added dimethylcarbamyl chloride (0.65 g). The mixture was refluxed for 24 hours under N2. TLC (silica gel, 10% MeOH/DCM) showed no starting material. The reaction was filtered and the filtrate concentrated in vacuo. Flash chromatography (silica gel) eluting with 5% acetone/5% MeOH/CH2Cl2 provided a residue which upon crystallization afforded 0.5 g of the product, m.p. 150° C.

1. temperatureThe mixture was refluxed for 24 hours under N2
2. filtrationThe reaction was filtered
3. concentrationthe filtrate concentrated in vacuo
4. washFlash chromatography (silica gel) eluting with 5% acetone/5% MeOH/CH2Cl2
5. customprovided a residue which
6. customupon crystallization