HRID1896914

反应详情

EQUATION

反应方程式

HRID 1896914 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of methyl N-(1-1,4-dioxaspiro[4.5]decan-8-ylpropyl)carbamate (as prepared in the previous step, 39 mg, 0.15 mmol, 1.00 equiv) in CH3CN (5 mL) and HCl (2M, 1 mL) was stirred for 2 h at room temperature. The resulting mixture was concentrated under vacuum. The residue was diluted with 10 mL of aq. sodium bicarbonate (1M). The resulting solution was extracted with 2×20 mL of dichloromethane. The organic layers were combined, dried over anhydrous sodium sulfate and concentrated under vacuum to give the title compound as a yellow oil.

WORKUP

后处理

  1. concentrationThe resulting mixture was concentrated under vacuum
  2. additionThe residue was diluted with 10 mL of aq. sodium bicarbonate (1M)
  3. extractionThe resulting solution was extracted with 2×20 mL of dichloromethane
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under vacuum