HRID1848469

反应详情

EQUATION

反应方程式

HRID 1848469 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of tert-butyl 2-(4-chloro-5-oxo-2,5-dihydrofuran-3-yl)-1-oxo-2,8-diazaspiro[4.5]decane-8-carboxylate (2.26 g, 6.09 mmol) in methylene chloride (10 mL) was added trifluoroacetic acid (9.39 mL, 122 mmol) and the resulting solution was stirred at rt for 1 h. After removing the volatiles, the residue was partitioned between methylene chloride (100 mL) and 1N sodium hydroxide (100 mL). The alkaline phase was extracted with methylene chloride (2×100 mL). The combined organic phase was dried over sodium sulfate and concentrated to give 2-(4-chloro-5-oxo-2,5-dihydrofuran-3-yl)-2,8-diazaspiro[4.5]decan-1-one. LC/MS: (M+1)+: 271.07, 272.96.

WORKUP

后处理

  1. customAfter removing the volatiles
  2. customthe residue was partitioned between methylene chloride (100 mL) and 1N sodium hydroxide (100 mL)
  3. extractionThe alkaline phase was extracted with methylene chloride (2×100 mL)
  4. dry with materialThe combined organic phase was dried over sodium sulfate
  5. concentrationconcentrated