HRID1443380

反应详情

EQUATION

反应方程式

HRID 1443380 的结构方程式

PROCEDURE

实验过程

Triflouroacetic acid (TFA) (4 mL) was cooled in a test tube to about 0° C. To the cool solvent was then added the product prepared in Step B (0.75 g, 2 mmol) above. The reaction mixture was allowed to warm to room temperature over about 45 minutes. Excess TFA was removed under a stream of N2 gas. The residue was partitioned between dichloromethane (15 mL) and saturated NaHCO3. The aqueous phase was then re-extracted with a second portion of dichloromethane and the organic phases combined, dried over MgSO4 and filtered, to yield the title compound in dichloromethane solution. The filtrate was used in the next step without further purification or isolation.

WORKUP

后处理

  1. customExcess TFA was removed under a stream of N2 gas
  2. customThe residue was partitioned between dichloromethane (15 mL) and saturated NaHCO3
  3. extractionThe aqueous phase was then re-extracted with a second portion of dichloromethane
  4. dry with materialdried over MgSO4
  5. filtrationfiltered