تفاعل #1769052

معادلة التفاعل

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

ethanol

thionyl chloride

→

product

المردود 63.0%

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

المردود 63.0%

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةby heating
2. 2
   درجة الحرارةThe resulting solution was refluxed 20 h
3. 3
   أخرىevaporated to dryness in vacuo
4. 4
   workup.ADDITIONdry THF (10 ml) was added
5. 5
   أخرىcrystallization

الإجراء التجريبي

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 20 h 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.

المصدر