HRID479495

反应详情

EQUATION

反应方程式

HRID 479495 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of Example 38A (183 mg, 0.650 mmol) and phenyl isocyanate (77 mg, 0.65 mmol) in THF (4 mL) at ambient temperature was treated with triethylamine (0.93 mL, 0.66 mmol). The mixture was stirred for 10 hours, diluted with ethyl acetate (20 mL), and washed with aqueous NH4Cl (10 mL), water (10 mL), and brine (5 mL). The organic portion was dried (MgSO4), filtered, and concentrated to provide an oily residue which was purified by flash chromatography (elution with 5% methanol/CH2Cl2) to provide 151 mg of the desired product as an off-white solid.

WORKUP

后处理

  1. washwashed with aqueous NH4Cl (10 mL), water (10 mL), and brine (5 mL)
  2. dry with materialThe organic portion was dried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customto provide an oily residue which
  6. customwas purified by flash chromatography (elution with 5% methanol/CH2Cl2)