HRID1711092

反应详情

EQUATION

反应方程式

HRID 1711092 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 331 (607 mg, 2.18 mmol) and IN NaOH (5.5 mL) in methanol (15 mL) was heated at 45° C. for 16 h under nitrogen. The reaction mixture was allowed to cool to room temperature; it was then concentrated, diluted with water, and washed with hexanes. The aqueous layer was collected, acidified with 3N HCl and extracted twice with AcOEt. The organic extract was dried over anhydrous magnesium sulfate, filtered, and concentrated to afford title compound 332 (400 mg, 94% yield, mono-hydrate) as an orange sticky solid. LCMS: 201.1 (M+Na)+.

WORKUP

后处理

  1. concentrationit was then concentrated
  2. additiondiluted with water
  3. washwashed with hexanes
  4. customThe aqueous layer was collected
  5. extractionextracted twice with AcOEt
  6. extractionThe organic extract
  7. dry with materialwas dried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated