تفاعل #1740889
ord-4ab2bac8a4354d3d9ca040e5cec9d1c8
معادلة التفاعل
1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride
methanol
thionyl chloride
→
white crystals
المردود 60.0%
1,4,5,6-Tetrahydro-5-methoxycarbonylpyrimidine Hydrochloride
المردود 60.0%
الكواشف
لا شيء
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةThe resulting solution was refluxed
- 2workup.STIRRINGwith stirring for 18 hours
- 3أخرىevaporated in vacuo to white solids
- 4أخرىThe crude product was recrystallized from anhydrous methanol
الإجراء التجريبي
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.