反应 #4550

反应方程式

1-bromoctane

(s)-4-[5-(6-methyl octyl)-2-pyrimidinyl]phenol

sodium hydride

→

(s)-2-[4-n-octyloxyphenyl]-5-[6-methyloctyl]pyrimidine

溶剂

N,N-dimethylformamide

N,N-dimethylformamide

反应条件

后处理

1. 1
   其他equipped with a cooling tube
2. 2
   其他for 30 minutes
3. 3
   其他to react for 7 hours at 90° C
4. 4
   其他After the reaction
5. 5
   萃取extract the product with ethyl acetate
6. 6
   洗涤The organic layer is thoroughly washed with water
7. 7
   其他dried
8. 8
   其他the organic solvent is evaporated
9. 9
   其他removed
10. 10
    其他the impure product is obtained
11. 11
    其他recrystallized

实验过程

Pour 0.33 g of sodium hydride (about 50% oil suspension), 3 ml of dry N,N-dimethylformamide into a 30 ml three-mouth flask equipped with a cooling tube, thermometer, dripping funnel, and calcium chloride tube. Next, slowly drip 1.71 g of optically active (s)-4-[5-(6-methyl octyl)-2-pyrimidinyl]phenol which is dissolved in 6 ml of dry N,N-dimethylformamide, into the flask at room temperature. Furthermore, after reacting it for 30 minutes, add 1.10 g of 1-bromoctane, allow to react for 7 hours at 90° C. After the reaction, pour the mixture into ice water, then extract the product with ethyl acetate. The organic layer is thoroughly washed with water, dried, the organic solvent is evaporated and removed, and then the impure product is obtained. This impure product is refined with silica gel chromatography, and recrystallized to obtain 1.3 g of optically active (s)-2-[4-n-octyloxyphenyl]-5-[6-methyloctyl]pyrimidine.

来源