반응 #321881

반응 방정식

4,7-dichloroquinoline

1,2-diamino-2-methylpropane

→

N1 -(7-Chloro-quinolin-4-yl)-2-methyl-propane-1,2-diamine

용매

N-methyl-2-pyrrolidone

반응 조건

후처리

1. 1
   기타Thereafter, the solvent was evaporated in a vacuum
2. 2
   추출the mixture was extracted once with 200 ml of ethyl acetate and twice with 100 ml of ethyl acetate each time
3. 3
   workup.ADDITIONsubsequently treated with about 170 ml of 30% potassium hydroxide solution until the pH
4. 4
   기타Thereby, 88 g of N1 -(7-chloro-quinolin-4-yl)-2-methyl-propane-1,2-diamine separate out in crystalline form

실험 절차

52.8 g of 4,7-dichloroquinoline and 30.85 g of 1,2-diamino-2-methylpropane were stirred in 530 ml of N-methyl-2-pyrrolidone under argon at 150° C. for 5 hours. Thereafter, the solvent was evaporated in a vacuum and the residue was taken up in 1250 ml of water. After adjustment to pH 1 using conc. hydrochloric acid, the mixture was extracted once with 200 ml of ethyl acetate and twice with 100 ml of ethyl acetate each time, and subsequently treated with about 170 ml of 30% potassium hydroxide solution until the pH reached 12. Thereby, 88 g of N1 -(7-chloro-quinolin-4-yl)-2-methyl-propane-1,2-diamine separate out in crystalline form; m.p.: 169°-171° C.

출처