반응 #40628

반응 방정식

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

수율 102.0%

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

수율 102.0%

용매

dichloromethane

반응 조건

후처리

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

실험 절차

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.

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