反应 #2195505

ord-e71af8df398141858e4518bc0f82dc60

反应方程式

CC(C)(C)[Si](C)(C)OC1CC(=O)OC(=O)C1
4-(tert-butyldimethylsilyloxy)dihydro-2H-pyran-2,6(3H)-dione
[NH4+].[OH-]
ammonium hydroxide
N
ammonia
CC(C)(C)[Si](C)(C)OC1CC(=O)NC(=O)C1
title compound
CC(C)(C)[Si](C)(C)OC1CC(=O)NC(=O)C1
4-(tert-Butyldimethylsilyloxy)piperidine-2,6-dione

溶剂

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度Cool in an ice/water bath
  2. 2
    其他Cap the pressure tube
  3. 3
    温度Cool the mixture
  4. 4
    浓缩concentrate in vacuo
  5. 5
    其他Purify the residue by silica gel chromatography

实验过程

Dissolve 4.1 mmol of 4-(tert-butyldimethylsilyloxy)dihydro-2H-pyran-2,6(3H)-dione (Nagao Y et al., Chem. Lett. 1990 9: 1503) in 10 mL of dioxane in a pressure tube. Cool in an ice/water bath, add 15 mL of saturated ammonium hydroxide and treat with gaseous ammonia via bubbler for about 10 min. Cap the pressure tube and heat in a 100° C. oil bath for 17 h. Cool the mixture and concentrate in vacuo. Purify the residue by silica gel chromatography using ethyl acetate/hexanes eluant to yield the title compound.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07514068B2uspto-grants-2009_04