HRID460348

反应详情

EQUATION

反应方程式

HRID 460348 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 6-methoxy-5-oxiranylmethoxy-indan-1-one (Intermediate M, 2.5 g, 0.0106 mole) and pyrrolidine (0.9 mL, 0.011 mole) was stirred in 50 mL of DME at 50° C. for 5 hrs under Argon. Then, 150 mL of ethyl acetate was added and the solution washed with water (2×). Following extraction with 2N HCl, the aqueous acidic layer was made basic with 3N NaOH and extracted with ethyl acetate. The ethyl acetate extracts were washed with brine, dried over sodium sulfate and the solvent removed in vacuo. The resulting residue was triturated with diethyl ether to yield the title compound. MS m/z 306 (M+H)+.

WORKUP

后处理

  1. washthe solution washed with water (2×)
  2. extractionextraction with 2N HCl
  3. extractionextracted with ethyl acetate
  4. washThe ethyl acetate extracts were washed with brine
  5. dry with materialdried over sodium sulfate
  6. customthe solvent removed in vacuo
  7. customThe resulting residue was triturated with diethyl ether