HRID627198

反应详情

EQUATION

反应方程式

HRID 627198 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (2S)-tert-butyl 5-(N-(allyloxy)-2-nitrophenylsulfonamido)-4-(2-amino-2-oxoethyl)-2-carbamoyl-5,6-dihydropyridine-1(2H)-carboxylate (Intermediate 175, 1.36 g, 2.52 mmol) and potassium carbonate (1.742 g, 12.60 mmol) in acetonitrile (20.0 mL) at 0° C. was added benzenethiol (1.389 g, 12.60 mmol). The mixture was stirred at room temperature for 15 hours. The reaction mixture was concentrated and the resulting residue was triturated with DCM. The solids were removed by filtration. The filtrate was concentrated to a pale yellow film, which was subjected to silica gel column eluting with 0-50% MeOH/DCM to give a pale yellow solid, 330 mg, 36.9%.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. customthe resulting residue was triturated with DCM
  3. customThe solids were removed by filtration
  4. concentrationThe filtrate was concentrated to a pale yellow film, which
  5. washeluting with 0-50% MeOH/DCM
  6. customto give a pale yellow solid, 330 mg, 36.9%