HRID1511368

反应详情

EQUATION

反应方程式

HRID 1511368 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
35 °C

PROCEDURE

实验过程

To a stirring solution of (R,Z)—N-(4-bromo-2-chlorobenzylidene)-2-methylpropane-2-sulfinamide (1370 mg, 4246 μmol) and (trifluoromethyl)trimethylsilane (943 μl, 6369 μmol) in DMF (5 mL) was added 1,3-bis(1-adamantyl)imidazol-2-ylidene (143 mg, 425 μmol). Reaction stirred at 35° C. for 18 h then quenched with sat NH4Cl (10 mL). Reaction partitioned between EtOAc (40 mL) and 5% NaHCO3 (10 mL). Organic dried over MgSO4, concentrated to and oil from toluene, then purified on silica (80 g) eluting with 20>30% EtOAc/Hex. Product isolated as a white solid.

WORKUP

后处理

  1. customReaction
  2. customthen quenched with sat NH4Cl (10 mL)
  3. customReaction
  4. custompartitioned between EtOAc (40 mL) and 5% NaHCO3 (10 mL)
  5. dry with materialOrganic dried over MgSO4
  6. concentrationconcentrated to and oil from toluene
  7. custompurified on silica (80 g)
  8. washeluting with 20>30% EtOAc/Hex
  9. customProduct isolated as a white solid