Hydrochloric Acid → 3-Amino-N-{[5-chloro-2-(methoxypropyl)-1-oxidopyridin-4-yl]methyl}-N-cyclopropyl-2-{4-[2-(2,6-dichloro-4-methylphenoxy)ethoxy]benzyl}propanamide

HRID 561883Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 561883
[Cl:1][C:2]1[C:3]([CH2:14][N:15]([CH:48]2[CH2:50][CH2:49]2)[C:16](=[O:47])[CH:17]([CH2:27][C:28]2[CH:33]=[CH:32][C:31]([O:34][CH2:35][CH2:36][O:37][C:38]3[C:43]([Cl:44])=[CH:42][C:41]([CH3:45])=[CH:40][C:39]=3[Cl:46])=[CH:30][CH:29]=2)[CH2:18][NH:19]C(=O)OC(C)(C)C)=[CH:4][C:5]([CH2:9][CH2:10][CH2:11][O:12][CH3:13])=[N+:6]([O-:8])[CH:7]=1.Cl>C(Cl)Cl>[NH2:19][CH2:18][CH:17]([CH2:27][C:28]1[CH:33]=[CH:32][C:31]([O:34][CH2:35][CH2:36][O:37][C:38]2[C:43]([Cl:44])=[CH:42][C:41]([CH3:45])=[CH:40][C:39]=2[Cl:46])=[CH:30][CH:29]=1)[C:16]([N:15]([CH2:14][C:3]1[C:2]([Cl:1])=[CH:7][N+:6]([O-:8])=[C:5]([CH2:9][CH2:10][CH2:11][O:12][CH3:13])[CH:4]=1)[CH:48]1[CH2:50][CH2:49]1)=[O:47]

Komponenten

4

Versuchsvorschrift

To a CH2Cl2 solution (0.07 M) of tert-butyl (3-[{[5-chloro-2-(methoxypropyl)-1-oxidopyridin-4-yl]methyl}(cyclopropyl)amino]-2-{4-[2-(2,6-dichloro-4-methylphenoxy)ethoxy]benzyl}-3-oxopropyl)carbamate from the previous step (1 eq.) was added HCl (4.0 M dioxane solution, 30 eq.). The resulting solution was stirred at RT for 16 h. Following the removal of the volatiles in vacuo, the resulting residue was directly subjected to column chromatography (SiO2, 95:5 (v/v) CH2Cl2: 2.0 M NH3 in MeOH) to afford the title compound as an oil. MS (ESI+): 651.

Aufarbeitung

  1. customthe removal of the volatiles in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-4261ab71dd824d9599905af6b70d1698
Quelldatensatz
uspto-grants-2011_11
Patentnummer
US08063105B2

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