Acetate-hydrochloric acid → HCID 11634767, Verbindung

HRID 1892827Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1892827
[NH2:1][C:2]1[CH:14]=[C:13]([C@H:15]([NH:18][C:19]([N:21]2[C:27](=[O:28])[C@@H:26]([CH2:29][C:30]3[CH:35]=[C:34]([Cl:36])[CH:33]=[CH:32][C:31]=3[O:37][CH3:38])[CH2:25][N:24](CC3C(OC)=CC(OC)=CC=3OC)[C:23](=[O:52])[CH2:22]2)=[O:20])[CH2:16][CH3:17])[CH:12]=[CH:11][C:3]=1[C:4]([O:6]C(C)(C)C)=[O:5].Cl.C(O)(=O)C>>[NH2:1][C:2]1[CH:14]=[C:13]([C@H:15]([NH:18][C:19]([N:21]2[C:27](=[O:28])[C@@H:26]([CH2:29][C:30]3[CH:35]=[C:34]([Cl:36])[CH:33]=[CH:32][C:31]=3[O:37][CH3:38])[CH2:25][NH:24][C:23](=[O:52])[CH2:22]2)=[O:20])[CH2:16][CH3:17])[CH:12]=[CH:11][C:3]=1[C:4]([OH:6])=[O:5]

Komponenten

3

Edukt 2

HCID 22641269Acetate-hydrochloric acidHCID 66934849HCID 66934849, Verbindung

Produkt 1

HCID 11634767HCID 11634767, VerbindungAusbeute 28 %

Versuchsvorschrift

(Step 2) To tert-butyl 2-amino-4-[(1R)-1-({[(6S)-6-(5-chloro-2-methoxybenzyl)-3,7-dioxo-4-(2,4,6-trimethoxybenzyl)-1,4-diazepan-1-yl]carbonyl}amino)propyl]benzoate (1.47 g), 1M hydrogen chloride/acetic acid solution (15 ml) was added and the mixture was stirred at room temperature for 20 hours. The reaction solution was concentrated, then the residue was purified by silica gel column chromatography (chloroform/ethyl acetate/methanol/acetic acid=8/8/1/0.1) to obtain the title compound (0.28 g).

Aufarbeitung

  1. concentrationThe reaction solution was concentrated
  2. customthe residue was purified by silica gel column chromatography (chloroform/ethyl acetate/methanol/acetic acid=8/8/1/0.1)

Quellen und Nachweise

ORD-Eintrag
ord-1eb4ebe396984d62b10945b58c72c8fd
Quelldatensatz
uspto-grants-2013_08
Patentnummer
US08507714B2

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