반응 #446030

반응 방정식

sodium methoxide

6-cyclopropylpyridine-2,3-dicarboxylic acid diethyl ester

2-amino-2,3-dimethylbutyramide

→

6-cyclopropyl-2-(5-isopropyl-5-methyl-4-oxoimidazolin-2-yl)-pyridinecarboxylic acid

수율 57.9%

용매

methanol

ethanol

반응 조건

후처리

1. 1
   온도under reflux for 3 hours
2. 2
   농축It is then concentrated
3. 3
   workup.DISSOLUTIONthe residue is dissolved in a small amount of water
4. 4
   추출the solution is extracted three times with 150 ml of ethyl acetate each time
5. 5
   건조The organic phase is dried over magnesium sulphate
6. 6
   여과filtered
7. 7
   농축concentrated
8. 8
   기타The residue crystallises from ether/hexane 1:2

실험 절차

10 g of 30% sodium methoxide in methanol are added to a solution of 6 g of 6-cyclopropylpyridine-2,3-dicarboxylic acid diethyl ester and 3 g of 2-amino-2,3-dimethylbutyramide in 100 ml of ethanol and the reaction mixture is boiled under reflux for 3 hours. It is then concentrated, the residue is dissolved in a small amount of water, and the solution is saturated with sodium chloride. The pH is then adjusted to 4 with concentrated hydrochloric acid and the solution is extracted three times with 150 ml of ethyl acetate each time. The organic phase is dried over magnesium sulphate, filtered and concentrated. The residue crystallises from ether/hexane 1:2. In this manner 4 g of 6-cyclopropyl-2-(5-isopropyl-5-methyl-4-oxoimidazolin-2-yl)-pyridinecarboxylic acid having a melting point of 118°-121° are obtained.

출처