HRID238150

反应详情

EQUATION

反应方程式

HRID 238150 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(RS)—S-(4-aminophenyl)-N-(ethoxycarbonyl)-S-methylsulfoximide (10 g, 42 mmol), 5-bromo-2-chloro-4-methylsulfanyl-pyrimidine (10 g, 42 mmol) and 5M HCl (8 mL) in dioxane is stirred at 60° C. in 90% acetonitrile-water (250 mL) for 36 h. TLC indicates almost complete consumption of starting sulfoximine. The reaction mixture is poured into 800 mL of aq. NaHCO3, the pasty precipitate filtered, washed with 70 mL of EtOAc, then crude material (7.5 g) is recrystallized from boiling EtOH (200 mL) to yield 6 g (35%).

WORKUP

后处理

  1. customconsumption of starting sulfoximine
  2. additionThe reaction mixture is poured into 800 mL of aq. NaHCO3
  3. filtrationthe pasty precipitate filtered
  4. washwashed with 70 mL of EtOAc
  5. customcrude material (7.5 g) is recrystallized
  6. customto yield 6 g (35%)