반응 #570803

반응 방정식

5-(1,3-Dioxepan-2-yl)-2,3-pyridinedicarboxylic acid, dimethyl ester

2-amino-2,3-dimethylbutyramide

potassium tert-butoxide

→

title compound

수율 57.2%

5-(1,3-Dioxepan-2-yl)-2-(4-isopropyl-4-methyl-5-oxo-2-imidazolin-2-yl)nicotinic acid

수율 57.2%

용매

toluene

toluene

water

water

반응 조건

후처리

1. 1
   온도The mixture is heated for 3 hours from 60° to 70° C
2. 2
   농축the mixture is concentrated in vacuo
3. 3
   기타to give an oil
4. 4
   세척washed with ether
5. 5
   추출extracted with methylene chloride
6. 6
   건조The combined methylene chloride extracts are dried over anhydrous magnesium sulfate
7. 7
   농축concentrated in vacuo

실험 절차

5-(1,3-Dioxepan-2-yl)-2,3-pyridinedicarboxylic acid, dimethyl ester (0.9 g, 0.00305 mol) in toluene is added to 2-amino-2,3-dimethylbutyramide (0.4 g, 0.00305 mol) and potassium tert-butoxide (0.69 g, 0.0061 mol) in toluene. The mixture is heated for 3 hours from 60° to 70° C. The reaction mixture is cooled to room temperature, water is added and the mixture is concentrated in vacuo to give an oil. The oil is diluted with water and washed with ether. The aqueous solution is acidified to pH 3.1 with 2 normal hydrochloric acid solution and extracted with methylene chloride. The combined methylene chloride extracts are dried over anhydrous magnesium sulfate and concentrated in vacuo to give the title compound as a white solid (0.63 g, 57%) mp 60°-69° C., identified by IR and NMR spectral analyses.

출처