تفاعل #69756

معادلة التفاعل

ethyl 2-acetyl-3-ethoxy-2-propenoate

((amino(imino)methyl)-sulfanyl)methane

triethylamine

→

solid

المردود 81.0%

4-Methyl-2-methylsulfanyl-pyrimidine-5-carboxylic acid ethyl ester

المردود 81.0%

المذيبات

EtOH

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةat reflux for 48 hours
2. 2
   أخرىThen reaction mixture
3. 3
   تركيزwas concentrated
4. 4
   workup.ADDITIONdiluted with water
5. 5
   أخرىThe biphasic mixture was transferred into a separatory funnel
6. 6
   استخلاصextracted with DCM
7. 7
   استخلاصOrganic extract
8. 8
   غسيلwas washed with water
9. 9
   أخرىdried
10. 10
    ترشيحfiltered
11. 11
    تركيزconcentrated
12. 12
    أخرىThe product was purified by crystallization from ethanol/water

الإجراء التجريبي

Equimolar quantities of ethyl 2-acetyl-3-ethoxy-2-propenoate 1 (20.0 g, 107 mmol), ((amino(imino)methyl)-sulfanyl)methane 2 (9.68 g, 107 mmol) and triethylamine (10.8 g, 107 mmol) in EtOH (100 mL) were stirred at reflux for 48 hours. Then reaction mixture was concentrated and diluted with water. The biphasic mixture was transferred into a separatory funnel and extracted with DCM. Organic extract was washed with water, dried, filtered, and concentrated. The product was purified by crystallization from ethanol/water to yield in a colorless solid (18.4 g, 86.7 mmol, 81%).

المصدر