반응 #1740889

반응 방정식

1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride

methanol

thionyl chloride

→

white crystals

수율 60.0%

1,4,5,6-Tetrahydro-5-methoxycarbonylpyrimidine Hydrochloride

수율 60.0%

반응 조건

후처리

1. 1
   온도The resulting solution was refluxed
2. 2
   workup.STIRRINGwith stirring for 18 hours
3. 3
   기타evaporated in vacuo to white solids
4. 4
   기타The crude product was recrystallized from anhydrous methanol

실험 절차

1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride (6.34 g, 38.5 mmol) was dissolved in anhydrous methanol (200 ml) with stirring, and thionyl chloride (2.74 ml, 38.5 mmol) was added dropwise. The resulting solution was refluxed with stirring for 18 hours, then evaporated in vacuo to white solids. The crude product was recrystallized from anhydrous methanol to yield 4.12 g (60%) white crystals, mp 160°-164° C. Calculated: C 40.34, H 6.21, N 15.69; found: C 40.17, H 6.41, N 15.73.

출처