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Triethylamine → HCID 68711084, Verbindung

HRID 638806
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 638806
[C:1]([O:5][C:6]([NH:8][CH2:9][C:10]([OH:12])=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C.F[P-](F)(F)(F)(F)F.C[NH2+]C.[Cl:30][C:31]1[CH:32]=[C:33]([CH:41]=[CH:42][C:43]=1[Cl:44])[CH2:34][N:35]1[CH2:38][CH:37]([CH2:39][NH2:40])[CH2:36]1>ClCCl>[C:1]([O:5][C:6](=[O:7])[NH:8][CH2:9][C:10](=[O:12])[NH:40][CH2:39][CH:37]1[CH2:38][N:35]([CH2:34][C:33]2[CH:41]=[CH:42][C:43]([Cl:44])=[C:31]([Cl:30])[CH:32]=2)[CH2:36]1)([CH3:2])([CH3:3])[CH3:4]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 8471TriethylamineHCID 78288N-(tert-butoxycarbonyl)glycineHCID 18551499Dimethyl-ammonium hexafluorophosphateHCID 68712490HCID 68712490, Verbindung

Produkt 1

HCID 68711084HCID 68711084, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344
Dichloromethane
Lösungsmittel
2×

Versuchsvorschrift

A solution of tert-Butoxycarbonylamino-acetic acid (1.88 g, 10.7 mmol) in dichloromethane (15 ml) is treated with triethylamine (1.5 ml, 10.7 mmol) and [Dimethylamino-[1,2,3]-triazolo-[4,5-b]pyridin-3-yloxy)-methylene]-dimethyl-ammonium hexafluoro phosphate (4.06 g, 10.7 mmol) and stirred for 5 minutes. To the reaction mixture is added a solution of C-[1-(3,4-Dichloro-benzyl)-azetidin-3-yl]-methylamine (2.64 g, 10.7 mmol) in dichloromethane (15 ml) with stirring for a further 3 hours. The reaction mixture is partitioned between dichloromethane and saturated sodium bicarbonate solution, the organic phase is washed with brine, dried over magnesium sulphate and evaporated. The crude product is purified by chromatography over flash silica eluting with 7% methanol in dichloromethane to afford the title compound.

Aufarbeitung

  1. stirringwith stirring for a further 3 hours
  2. customThe reaction mixture is partitioned between dichloromethane and saturated sodium bicarbonate solution
  3. washthe organic phase is washed with brine
  4. dry with materialdried over magnesium sulphate
  5. customevaporated
  6. customThe crude product is purified by chromatography over flash silica eluting with 7% methanol in dichloromethane

Quellen und Nachweise

ORD-Eintrag
ord-8c20a0d7fbad47a681ab0069aaa0dfa2
Quelldatensatz
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07691841B2

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