反应详情

To a mechanically stirred 16° C. pyridine (270 mL) solution of 1-[4-phenylmethoxy-3-aminophenyl]ethanone (57.4 g, 238 mmol) under N2, was added methanesulfonyl chloride (18.6 mL, 240 mmol). After 39 minutes, the completed reaction was quenched with 1.8 L H2O and the resulting suspension stirred for ~2 hours before filtration. The collected solids were washed with H2O (2×250 mL=500 mL) and partially air dried. These solids were dissolved in CHCl3 (450 mL), the aqueous phase removed and heptane (475 mL) added with stirring. The resulting fine suspension was filtered after ~15 minutes, washed with hexane and dried in vacuo at 55° C. to give 59 g (78%) of the title compound.

1. customthe completed reaction
2. customwas quenched with 1.8 L H2O
3. washThe collected solids were washed with H2O (2×250 mL=500 mL) and partially air
4. customdried
5. dissolutionThese solids were dissolved in CHCl3 (450 mL)
6. customthe aqueous phase removed
7. additionheptane (475 mL) added
8. stirringwith stirring
9. filtrationThe resulting fine suspension was filtered after ~15 minutes
10. washwashed with hexane
11. customdried in vacuo at 55° C.