HRID12350

反应详情

EQUATION

反应方程式

HRID 12350 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. concentrationthe solution was concentrated
  2. dissolutionthe crude residue was redissolved in dichloromethane (10 mL)
  3. waitAfter 15 h
  4. customthe reaction mixture was partitioned between water and dichloromethane
  5. customthe organic layer was separated
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated