HRID1802462

反应详情

EQUATION

反应方程式

HRID 1802462 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 9H-fluoren-9-ylmethyl[5-(chlorosulfonyl)-2,4-dimethylphenyl]carbamate (1.0 g, 2.3 mmol) in CH2Cl2 (23 mL) was added 1-pyridin-3-ylmethanamine (0.46 mL, 4.5 mmol) and pyridine (0.55 mL, 6.8 mmol). The bright yellow solution was then stirred at room temperature overnight and then quenched by the addition of sat. aq. NaHCO3 solution. The reaction was extracted with EtOAc and the organic extracted were dried over Na2SO4 and concentrated in vacuo. Purification by silica gel column chromatography (0-5% MeOH/DCM) afforded the title compound.

WORKUP

后处理

  1. customquenched by the addition of sat. aq. NaHCO3 solution
  2. extractionThe reaction was extracted with EtOAc
  3. extractionthe organic extracted
  4. dry with materialwere dried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. customPurification by silica gel column chromatography (0-5% MeOH/DCM)