反应详情

A cooled (0° C.) solution of 4-[(3-amino-2-hydroxypropyl)oxy]benzonitrile (from step (ii) above; 44.6 g, 0.23 mol) in THF:H,O (1.5 L of 1:1) was treated with di-tert-butyl dicarbonate (53 g, 0.24 mol). The mixture was stirred at rt overnight, after which NaCl was added and the resulting organic layer separated. The water layer was extracted with ether and the combined organics were dried and concentrated in vacuo. The resulting oil (70 g) was filtered through a plug of silica, and then crystallised from diethyl ether:di-iso-propyl ether to yield 50 g of the sub-title compound.

1. customthe resulting organic layer separated
2. extractionThe water layer was extracted with ether
3. customthe combined organics were dried
4. concentrationconcentrated in vacuo
5. filtrationThe resulting oil (70 g) was filtered through a plug of silica
6. customcrystallised from diethyl ether