反应 #657271

ord-88bdae61eb98419aa9d5aff4c9fe1234

反应方程式

CC1CCCC(C)N1CC(=O)O.Cl
(2,6-Dimethyl-piperidin-1-yl)-acetic acid hydrochloride
CC1CCCC(C)N1CC(=O)O.Cl
(2,6-Dimethyl-piperidine-1-yl)-acetic acid hydrochloride
O=C1CCC(=O)N1O
N-hydroxysuccinimide
CC1CCCC(C)N1CC(=O)ON1C(=O)CCC1=O
(2,6-Dimethyl-piperidine-1-yl)-acetic acid-(2,5-dioxo-pyrrolidine-1-yl)-ester

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤The residue was filtered
  2. 2
    其他the filtrate was evaporated in vacuo to dryness
  3. 3
    workup.DISSOLUTIONAfter dissolving the residue in 300 ml CH2Cl2
  4. 4
    洗涤the solution was washed with NaHCO3
  5. 5
    干燥dried over sodium sulphate
  6. 6
    其他the solvent was evaporated
  7. 7
    其他The compound was then recrystallised from diisopropylether (activated charcoal)

实验过程

12.60 g (60 mMol) (2,6-Dimethyl-piperidin-1-yl)-acetic acid hydrochloride (5), in 100 ml DMF, was added to 7.02 g (60 mMol) N-hydroxysuccinimide and 12.58 g (60 mMol) N,N-dicyclohexylcarbodiimide. The reaction mixture was stirred for 16 h at RT. The residue was filtered and the filtrate was evaporated in vacuo to dryness. After dissolving the residue in 300 ml CH2Cl2, the solution was washed with NaHCO3, dried over sodium sulphate and the solvent was evaporated. The compound was then recrystallised from diisopropylether (activated charcoal).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09023656B2uspto-grants-2015_05