1,3-Propanediamine, N1,N1,N3-trimethyl- → HCID 178483532, Verbindung

HRID 77099

Reaktionsgleichung

[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][CH:11]([C:14](O)=[O:15])[CH2:10][CH2:9]2)=[CH:4][C:3]=1[C:17]1[NH:21][C:20]2[CH:22]=[CH:23][C:24]([F:26])=[CH:25][C:19]=2[N:18]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[CH3:51][N:52]([CH3:58])[CH2:53][CH2:54][CH2:55][NH:56][CH3:57]>ClCCl>[CH3:51][N:52]([CH3:58])[CH2:53][CH2:54][CH2:55][N:56]([CH3:57])[C:14]([CH:11]1[CH2:10][CH2:9][N:8]([C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[C:3]([C:17]3[NH:21][C:20]4[CH:22]=[CH:23][C:24]([F:26])=[CH:25][C:19]=4[N:18]=3)[CH:4]=2)[CH2:13][CH2:12]1)=[O:15]

Komponenten

Reaktionsbedingungen

Temperatur: 35 °C

Versuchsvorschrift

Method H—Step a To a vial with 1-[4-Chloro-3-(5-fluoro-1H-benzoimidazol-2-yl)-phenyl]-piperidine-4-carboxylic acid (obtained as described in general method 3,4, step e) (0.10 g, 0.26 mmol) and HATU (0.10 g, 0.27 mmol) in dichloromethane (2 mL), TEA (0.07 mL, 0.54 mmol) and N,N,N′-trimethyl-1,3-propanediamine (0.32 mmol, 0.05 mL) were added. The reaction mixture was heated at 35° C. overnight, solvent was removed and the crude was purified by PrepHPLC and SCX column to obtain 0.06 g of the title compound (49%).

Aufarbeitung

customsolvent was removed
customthe crude was purified by PrepHPLC and SCX column

Quellen und Nachweise

ORD-Eintrag: ord-27ca3a58482c406992ccbeb17b6ca9cb
Quelldatensatz: uspto-grants-2014_09
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08835648B2

Verknüpfte Notizen

Wird geladen…