반응 #657271

ord-88bdae61eb98419aa9d5aff4c9fe1234

반응 방정식

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

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The residue was filtered
  2. 2
    기타the filtrate was evaporated in vacuo to dryness
  3. 3
    workup.DISSOLUTIONAfter dissolving the residue in 300 ml CH2Cl2
  4. 4
    세척the solution was washed with NaHCO3
  5. 5
    건조dried over sodium sulphate
  6. 6
    기타the solvent was evaporated
  7. 7
    기타The compound was then recrystallised from diisopropylether (activated charcoal)

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09023656B2uspto-grants-2015_05