Acetate-hydrochloric acid → HCID 11634767, Verbindung

HRID 554773Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 554773
[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-3bc9d176b6774663b188635823d29330
Quelldatensatz
uspto-grants-2011_11
Patentnummer
US08049006B2

Notizen zur Reaktion

Wird geladen…