反应详情

温度

75 °C

The mixture of (E)-1-[3-[[4-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]-2-butenyl]oxy]-4-benzyloxyphenyl]ethanone (5.5 g, 10.7 mmol), acetic acid (50 ml), and hydrochloric acid (6 ml) was heated at 75° C. for 2 hours. At the end of reaction, the solvent was reduced to about 20 ml on a rotary evaporator. The solution was poured into ice water (350 ml) and extracted with dichloromethane (3×250 ml). The dichloromethane solution was washed with brine and dried over Na2SO4. A solid formed on concentration of the solvent. This was collected by filtration (3.4 g). Recrystallization from hot methanol (443 ml) gave 1.82 g of (E)-1-[3-[[4-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]-2-butenyl]oxy]-4-hydroxyphenyl]ethanone hydrochloride as white crystals, 37.5%, m.p.=208°-210° C.

1. customAt the end of reaction
2. customthe solvent was reduced to about 20 ml on a rotary evaporator
3. additionThe solution was poured into ice water (350 ml)
4. extractionextracted with dichloromethane (3×250 ml)
5. washThe dichloromethane solution was washed with brine
6. dry with materialdried over Na2SO4
7. customA solid formed on concentration of the solvent
8. filtrationThis was collected by filtration (3.4 g)
9. customRecrystallization from hot methanol (443 ml)