反应详情

The entire isolated, crude and moist phenylsulfonylacetic acid methyl ester (V) was transferred to a 2-L Erlenmeyer flask and dissolved in 1 L (11.7 mol) of 40% aqueous methylamine. The reaction temperature rose to 30° C. The mixture was allowed to cool to ambient temperature, and was maintained at this temperature for an additional hour, followed by cooling overnight in a refrigerator. The precipitate product (IV) was removed by filtration. The filter cake was washed with 3×300 mL of cold water. Drying the recovered white solid at 60° C. at 30 torr over potassium hydroxide flakes for 27 h yielded 402.7 g of the methylacetamide (IV), 97.3% purity by HPLC, mp 106-109° C.

1. customrose to 30° C
2. temperaturewas maintained at this temperature for an additional hour
3. temperatureby cooling overnight in a refrigerator
4. customThe precipitate product (IV) was removed by filtration
5. washThe filter cake was washed with 3×300 mL of cold water
6. dry with materialDrying the recovered white solid at 60° C. at 30 torr over potassium hydroxide flakes for 27 h