Dicyclohexylcarbodiimide → HCID 11253866, Verbindung

HRID 2364930Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2364930
Cl.[CH:2]([N:5]([CH2:9][C:10]([OH:12])=[O:11])[CH:6]([CH3:8])[CH3:7])([CH3:4])[CH3:3].O[N:14]1[C:18](=[O:19])[CH2:17][CH2:16][C:15]1=[O:20].C1(N=C=NC2CCCCC2)CCCCC1>CN(C=O)C>[O:20]=[C:15]1[CH2:16][CH2:17][C:18](=[O:19])[N:14]1[O:11][C:10](=[O:12])[CH2:9][N:5]([CH:6]([CH3:7])[CH3:8])[CH:2]([CH3:3])[CH3:4]

Komponenten

5

Edukt 3

HCID 10868DicyclohexylcarbodiimideHCID 80170N-HydroxysuccinimideHCID 46735981Diisopropylamino-acetic acid hydrochloride

Produkt 1

HCID 11253866HCID 11253866, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

3.82 g (19.5 mMol) diisopropylamino-acetic acid hydrochloride (3), in 50 ml DMF, was added to 2.24 g (19.5 mMol) N-hydroxysuccinimide and 8.04 g (39 nMol) dicyclohexylcarbodiimide. The reaction mixture was stirred for 16 h at RT. The residue was filtered and the filtrate was evaporated in vacuum to dryness. After dissolving the residue in CH2Cl2, the solution was washed with NaHCO3, dried (sodium sulphate) and the solvent evaporated. The compound was then recrystallised from diisopropylether.

Aufarbeitung

  1. filtrationThe residue was filtered
  2. customthe filtrate was evaporated in vacuum to dryness
  3. dissolutionAfter dissolving the residue in CH2Cl2
  4. washthe solution was washed with NaHCO3
  5. dry with materialdried (sodium sulphate)
  6. customthe solvent evaporated
  7. customThe compound was then recrystallised from diisopropylether

Quellen und Nachweise

ORD-Eintrag
ord-e82303fbef3d496fbcc8564df4c013f7
Quelldatensatz
uspto-grants-2014_04
Patentnummer
US08697604B2

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