HRID1193363

反应详情

EQUATION

反应方程式

HRID 1193363 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-Benzyl-N-methyl-1,4-dioxaspiro[4.5]decan-8-amine (1.0 g, 3.83 mmol, 1.0 eq.) was dissolved in MeOH (12 ml); 6 M HCl solution (12 ml) was added at 0° C., and stirring was carried out for 16 hours at RT. After monitoring by TLC, the solvent was removed under reduced pressure and the residue was taken up in water (50 ml), adjusted to pH 8-9 with NaCHO3 (solid) and extracted with DCM (2×50 ml). The combined org. phases were washed with water and sat. NaCl solution (in each case 50 ml), dried over sodium sulfate and concentrated under reduced pressure and dried. The crude product was used in the next stage without being purified further. Yield: 74% (620 mg, 2.857 mmol)

WORKUP

后处理

  1. customthe solvent was removed under reduced pressure
  2. extractionextracted with DCM (2×50 ml)
  3. washphases were washed with water and sat. NaCl solution (in each case 50 ml),
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customdried
  7. customwithout being purified further