HRID8933

反应详情

EQUATION

反应方程式

HRID 8933 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 2,2,2-trifluoro-1-piperazin-1-yl-ethanone (515 mg, 2.83 mmol) in dry CH3CN (6 mL) was added allyl bromide (0.32 mL, 3.7 mmol) and powdered potassium carbonate (0.78 g, 5.65 mmol) and the mixture stirred overnight. The reaction was concentrated under reduced pressure, diluted with CH2Cl2 (30 mL) and water (30 mL) and the aqueous layer extracted with CH2Cl2 (2×20 mL). The combined organic extracts were dried (Na2SO4), filtered and concentrated in vacuo to afford the crude di-protected piperazine (0.554 g) which was used without further purification in the next reaction.

WORKUP

后处理

  1. concentrationThe reaction was concentrated under reduced pressure
  2. additiondiluted with CH2Cl2 (30 mL) and water (30 mL)
  3. extractionthe aqueous layer extracted with CH2Cl2 (2×20 mL)
  4. dry with materialThe combined organic extracts were dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo