تفاعل #164730

معادلة التفاعل

6-iodo-1-(2-methoxyethyl)-2-thioxo-2,3-dihydropyrimidin-4(1H)-one

diisopropylethylamine

iodomethane

→

title compound

المردود 43.1%

6-Iodo-1-(2-methoxyethyl)-2-(methylthio)pyrimidin-4(1H)-one

المردود 43.1%

المذيبات

MeCN

ظروف التفاعل

المعالجة

1. 1
   تركيزconcentrated in vacuo
2. 2
   أخرىThe residue was partitioned
3. 3
   أخرىThe layers were separated
4. 4
   غسيلthe organic layer was washed with brine (100 mL)
5. 5
   تجفيفdried over MgSO4
6. 6
   تركيزconcentrated in vacuo
7. 7
   أخرىThe resulting residue was purified by hot trituration with CH2Cl2/heptane

الإجراء التجريبي

To a stirring solution of 6-iodo-1-(2-methoxyethyl)-2-thioxo-2,3-dihydropyrimidin-4(1H)-one (9.00 g, 28.83 mmol) in MeCN (200 mL) was added diisopropylethylamine (5.0 mL, 28.83 mmol) and iodomethane (9.0 mL, 144.17 mmol). The reaction mixture was stirred at room temperature for 18 hours, and concentrated in vacuo. The residue was partitioned ortioned between CH2Cl2 (200 mL) and 1N aqueous HCl (100 mL). The layers were separated and the organic layer was washed with brine (100 mL), dried over MgSO4 and concentrated in vacuo. The resulting residue was purified by hot trituration with CH2Cl2/heptane to give the title compound (4.05 g, 43%) as a cream colored solid.

المصدر