반응 #4550

반응 방정식

1-bromoctane

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

sodium hydride

→

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

용매

N,N-dimethylformamide

N,N-dimethylformamide

반응 조건

후처리

1. 1
   기타equipped with a cooling tube
2. 2
   기타for 30 minutes
3. 3
   기타to react for 7 hours at 90° C
4. 4
   기타After the reaction
5. 5
   추출extract the product with ethyl acetate
6. 6
   세척The organic layer is thoroughly washed with water
7. 7
   기타dried
8. 8
   기타the organic solvent is evaporated
9. 9
   기타removed
10. 10
    기타the impure product is obtained
11. 11
    기타recrystallized

실험 절차

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.

출처