反应 #1702173

反应方程式

3-bromo-4,5-dihydroisoxazole

pyrollidine

sodium carbonate

water

→

3-(Pyrrolidin-1-yl)-4,5-dihydroisoxazole

溶剂

tert-butylmethyl ether

n-butanol

反应条件

后处理

1. 1
   其他sealed
2. 2
   温度to cool
3. 3
   洗涤The aqueous layer was washed with tert-butylmethyl ether (2×)
4. 4
   洗涤the combined organic layers were washed with brine
5. 5
   干燥dried over magnesium sulfate
6. 6
   浓缩concentrate
7. 7
   其他to provide a orange solid
8. 8
   其他that was purified
9. 9
   其他to provide III-59 as a white solid

实验过程

3-(Pyrrolidin-1-yl)-4,5-dihydroisoxazole III-59 was prepared in 1 step according to the following procedure: 3-bromo-4,5-dihydroisoxazole III-18 (1.0 equiv) was dissolved in n-butanol (0.64 M) followed by the addition of pyrollidine (1.2 equiv) and sodium carbonate (2.5 equiv). The reaction is the sealed and heated in an oil bath to 120° C. for 18 h after which it allowed to cool and then transferred to a separatory funnel with excess water and tert-butylmethyl ether. The aqueous layer was washed with tert-butylmethyl ether (2×) and the combined organic layers were washed with brine, dried over magnesium sulfate and concentrate to provide a orange solid that was purified using flash silica gel chromatography (gradient ethyl acetate/hexanes) to provide III-59 as a white solid. [M+H]+=345.4 m/z. Activity: C

来源