반응 #735425

반응 방정식

p-trifluoromethylaniline

phenolphthalein

sodium hydroxide methanol

α-bromoisovaleric acid

sodium hydroxide

→

N-(p-trifluoromethylphenyl)valine

용매

dimethylformamide

methanol

반응 조건

후처리

1. 1
   기타The alcohol is then removed
2. 2
   온도The reaction mixture is heated at 100° for 2 hours
3. 3
   세척washed with ether
4. 4
   추출extracted with chloroform (3×)
5. 5
   세척washed with brine
6. 6
   기타dried
7. 7
   농축concentrated in a rotoevaporator and solvent
8. 8
   기타removed under vacuum at about 50°

실험 절차

Two grams of α-bromoisovaleric acid (0.011 mole) dissolved in 10 ml of methanol is titrated to the phenolphthalein end point at 0° with 2 N sodium hydroxide/methanol. The alcohol is then removed and 10 ml of dimethylformamide and p-trifluoromethylaniline (3.54 g, 0.022 mole) added. The reaction mixture is heated at 100° for 2 hours and left at room temperature about 18 hours. The reaction mixture is poured into 50 ml of 0.1 N sodium hydroxide, washed with ether and the aqueous phase adjusted to pH 4 with conc. HCl and then extracted with chloroform (3×). The extracts are combined and washed with brine, dried, concentrated in a rotoevaporator and solvent removed under vacuum at about 50° to yield N-(p-trifluoromethylphenyl)valine.

출처