反应详情

温度

0 °C

A cooled (0° C.) solution of 4-[(3-hydroxypropyl)amino]benzonitrile (from step (a) above; 17 g, 96.5 mmol) in dry MeCN (195 mL) was treated with triethylamine (9.8 g, 96.5 mmol) and then p-toluenesulfonyl chloride (20.2 g, 106 mmol). The mixture was stirred at 0° C. for 90 minutes before being concentrated in vacuo. Water (200 mL) was added to the residue, and the aqueous solution was extracted with DCM. The organic phase was dried (Na2SO4), filtered and concentrated in vacuo. The resulting residue was purified by crystallisation from iso-propanol to yield 24.6 g (77%) of the sub-title compound.

1. concentrationbefore being concentrated in vacuo
2. additionWater (200 mL) was added to the residue
3. extractionthe aqueous solution was extracted with DCM
4. dry with materialThe organic phase was dried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe resulting residue was purified by crystallisation from iso-propanol