반응 #1740885

반응 방정식

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

ethanol

thionyl chloride

→

product

수율 63.0%

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

수율 63.0%

반응 조건

후처리

1. 1
   온도by heating
2. 2
   기타evaporated to dryness in vacuo
3. 3
   workup.ADDITIONdry THF (10 ml) was added
4. 4
   기타crystallization

실험 절차

1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride (1.5 g, 9.12 mmol) was dissolved in absolute ethanol (40 ml) by heating. The thionyl chloride (1.1 g, 9.16 mmol) was added dropwise with stirring. The resulting solution was refluxed 20h and then evaporated to dryness in vacuo. The residue was taken up in absolute methanol (5 ml) and dry THF (10 ml) was added to induce crystallization, giving 1.1 g (63%) product as white crystals, mp 125°-127° C. 300 MHz nmr confirmed the product. Microanalysis calc.: C 43.64, H 6.75, N 14.55; found: C, 43.43, H 6.58, N 14.40.

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