反应详情

To a stirred solution of 3-[[2-(4-morpholinyl)ethyl]amino]-1,2-benzisoxazol-6-ol (2 g) and copper(I)chloride (0.3 g) in EtOAc (60 ml) was added methyl isocyanate (0.5 g). After 3.5 hours TLC (silica gel, 10% MeOH/DCM) showed no starting material. The reaction was filtered through neutral alumina eluting with EtOAc (2 l) and the filtrate was concentrated in vacuo. Flash column chromatography (silica gel) eluting with 1:1:20 acetone/MeOH/DCM afforded a white solid which was recrystallized from EtOAc/pet. ether to yield 0.7 g of the expected product, m.p. 127°-128° C.

1. filtrationThe reaction was filtered through neutral alumina eluting with EtOAc (2 l)
2. concentrationthe filtrate was concentrated in vacuo
3. washFlash column chromatography (silica gel) eluting with 1:1:20 acetone/MeOH/DCM
4. customafforded a white solid which
5. customwas recrystallized from EtOAc/pet. ether