반응 #70979

반응 방정식

6-chloro-1,3-dimethyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidine-5-carbaldehyde

triethyl-amine

N-methylprop-2-en-1-amine

→

6-[Allyl(methyl)amino]-1,3-dimethyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidine-5-carbaldehyde

용매

ethanol

반응 조건

후처리

1. 1
   기타After evaporation of the solvent in vacuo, water (15 ml)
2. 2
   workup.ADDITIONwas added to the yellow oily residue
3. 3
   추출the mixture was extracted with dichloromethane (4×15 ml)
4. 4
   건조The combined organic phases were dried over anhydrous MgSO4
5. 5
   기타The solvent was evaporated in vacuo
6. 6
   기타the crude product was purified by crystallization from a mixture of cyclohexane:isopropyl alcohol (4:1)

실험 절차

To a stirred solution of 6-chloro-1,3-dimethyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidine-5-carbaldehyde (0.500 g, 2.47 mmol) and triethyl-amine (0.52 ml, 3.71 mmol) in dry ethanol (10 ml), N-methylprop-2-en-1-amine (0.36 ml, 3.71 mmol) was added under argon. The resulting mixture was stirred at room temperature under argon overnight. After evaporation of the solvent in vacuo, water (15 ml) was added to the yellow oily residue, and the mixture was extracted with dichloromethane (4×15 ml). The combined organic phases were dried over anhydrous MgSO4. The solvent was evaporated in vacuo, and the crude product was purified by crystallization from a mixture of cyclohexane:isopropyl alcohol (4:1).

출처