HRID133125

反应详情

EQUATION

反应方程式

HRID 133125 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A stirred solution of (±)-methyl 2′-oxo-3,4-dihydro-1H-spiro[naphthalene-2,3′-pyrrolidine]-6-carboxylate from Step F (50 mg, 0.193 mmol) and lithium hydroxide (24 mg, 0.578 mmol) in THF (3 mL) and H2O (1 mL) was heated at reflux for 5 h, then allowed to cool. The mixture was poured into 10% aqueous HCl (10 mL) and extracted with EtOAc (3×20 mL), and the combined organic extracts were dried over Na2SO4, filtered, and concentrated in vacuo. The residue was triturated with CH2Cl2 to give the title compound. MS: m/z=246 (M+1).

WORKUP

后处理

  1. temperatureat reflux for 5 h
  2. temperatureto cool
  3. extractionextracted with EtOAc (3×20 mL)
  4. dry with materialthe combined organic extracts were dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue was triturated with CH2Cl2