تفاعل #40628

معادلة التفاعل

Bromine

8-cyclohexyl-2-methylsulfanyl-5-oxo-5,6,7,8-tetrahydro-pyrido[2,3-d]pyrimidine-6-carboxylic acid ethyl ester

diisopropylethylamine

→

title compound

المردود 102.0%

8-Cyclohexyl-2-methylsulfanyl-5-oxo-5,8-dihydro-pyrido[2,3-d]pyrimidine-6-carboxylic acid ethyl ester

المردود 102.0%

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   تركيزthe solution was concentrated
2. 2
   workup.DISSOLUTIONthe crude residue was redissolved in dichloromethane (10 mL)
3. 3
   workup.WAITAfter 15 h
4. 4
   أخرىthe reaction mixture was partitioned between water and dichloromethane
5. 5
   أخرىthe organic layer was separated
6. 6
   تجفيفdried (MgSO4)
7. 7
   تركيزconcentrated

الإجراء التجريبي

Bromine (0.15 g, 0.94 mmol) was added to a solution of 8-cyclohexyl-2-methylsulfanyl-5-oxo-5,6,7,8-tetrahydro-pyrido[2,3-d]pyrimidine-6-carboxylic acid ethyl ester (0.28 g, 0.79 mmol) in dichloromethane (10 mL). After 5 min, the solution was concentrated and the crude residue was redissolved in dichloromethane (10 mL) and diisopropylethylamine (0.42 mL, 2.4 mmol) was added. After 15 h, the reaction mixture was partitioned between water and dichloromethane, the organic layer was separated, dried (MgSO4) and concentrated to provide 0.28 g (87%) of the title compound. Mass Spectrum (LCMS, ESI pos.) Calcd. For C17H21N3O3S: 347.13. found: (M+H) 348.3.

المصدر