反应 #2271698

反应方程式

N-[3-[3-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidiny]propoxy]phenyl]acetamide

NaOH

→

3-[3-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]propoxy]aniline

溶剂

hydrochloric acid

反应条件

后处理

1. 1
   其他prepared
2. 2
   其他resulted The reaction
3. 3
   温度was cooled to 0° C. in an ice bath
4. 4
   萃取The product was extracted with ethyl acetate (3×200 ml)
5. 5
   洗涤The ethyl acetate solution was washed with water, brine
6. 6
   干燥dried over Na2SO4
7. 7
   其他The solvent was removed The crude product
8. 8
   其他was purified on a flash chromatography column
9. 9
   其他The product thus obtained
10. 10
    其他Recrystallization from hot ethanol (50 ml)

实验过程

A stirred mixture of N-[3-[3-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidiny]propoxy]phenyl]acetamide (9.2 g, 22 mmol), prepared as described in the previous example, in 15% hydrochloric acid (110 ml) was heated at 100° C. for 2.5 hours until a homogeneous solution resulted The reaction was cooled to 0° C. in an ice bath and basified with 50% NaOH. The product was extracted with ethyl acetate (3×200 ml). The ethyl acetate solution was washed with water, brine, then dried over Na2SO4. The solvent was removed The crude product was purified on a flash chromatography column. The product thus obtained was a solid: 6.6 g (80%). Recrystallization from hot ethanol (50 ml) gave 3-[3-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]propoxy]aniline as off-white crystals: 3.46 g, m.p.=115°-117° C. ANALYSIS: Calculated for C21H24FN3O2: 68.27%C 6,55%H 11.37%N Found: 68.34%C 6.53%H 11.31%N

来源