反应详情

温度

0 °C

To a solution of 3-[4-(hydroxymethyl)phenoxy]phthalonitrile (900 mg, 3.9 mmol) prepared according to procedures described in literature, and triethylamine (0.75 ml, 5.8 mmol) in anhydrous CH2Cl2 (50 ml), kept at 0° C. under stirring and in an inert atmosphere, methylsulfonylchloride was added (0.33 ml, 4.3 mmol). The mixture was stirred at 0° C. for 1 hour, then it was diluted with CH2Cl2 (50 ml) and washed with 1% HCl solution (60 ml), then with brine (50 ml), the organic layer was dried on Na2SO4 and the solvent was evaporated. 1.1 g (93%) of the title compound were obtained as a viscous fluid that crystallized on standing.

1. customkept at 0° C.
2. additionwas added (0.33 ml, 4.3 mmol)
3. washwashed with 1% HCl solution (60 ml)
4. dry with materialwith brine (50 ml), the organic layer was dried on Na2SO4
5. customthe solvent was evaporated