HRID1501759

反应详情

EQUATION

反应方程式

HRID 1501759 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To tert-butyl 2-(5-oxo-2,5-dihydrofuran-3-yl)-2,9-diazaspiro[5.5]undecane-9-carboxylate (266 mg, 0.792 mmol) in DCM (2 mL) was added TFA (2 mL, 26.0 mmol) at 0° C. The reaction mixture was stirred at room temperature for 1 h, then concentrated under reduced pressure, then placed on the high vacuum. The residue was dissolved in MeOH and loaded onto a 2 g Bond Elut SCX column (pre-rinsed with MeOH). These were rinsed with MeOH, and the product was eluted via 2M NH3 in MeOH to afford 4-(2,9-diazaspiro[5.5]undecan-2-yl)furan-2(5H)-one. LC/MS: [(M+1)]+=237

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. dissolutionThe residue was dissolved in MeOH
  3. washloaded onto a 2 g Bond Elut SCX column (pre-rinsed with MeOH)
  4. washThese were rinsed with MeOH
  5. washthe product was eluted via 2M NH3 in MeOH