Trifluoroacetic acid → HCID 25050873, Verbindung

HRID 1020250Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1020250
[Br:1][C:2]1[CH:3]=[C:4]([CH2:8][N:9](CC2C=CC(OC)=CC=2OC)[C:10]([NH:12][C:13]2[S:14][CH:15]=[C:16]([CH2:18][O:19][CH2:20][CH2:21][O:22][CH3:23])[N:17]=2)=[O:11])[S:5][C:6]=1[Br:7].C(O)(C(F)(F)F)=O.C1(OC)C=CC=CC=1>O>[Br:1][C:2]1[CH:3]=[C:4]([CH2:8][NH:9][C:10]([NH:12][C:13]2[S:14][CH:15]=[C:16]([CH2:18][O:19][CH2:20][CH2:21][O:22][CH3:23])[N:17]=2)=[O:11])[S:5][C:6]=1[Br:7]

Komponenten

5

Edukt 3

HCID 6422Trifluoroacetic acidHCID 7519AnisoleHCID 86622751HCID 86622751, Verbindung

Produkt 1

HCID 25050873HCID 25050873, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Deprotection: The 1-(4,5-Dibromo-thiophen-2-ylmethyl)-1-(2,4-dimethoxy-benzyl)-3-[4-(2-methoxy-ethoxymethyl)-thiazol-2-yl]-urea was treated with TFA followed by the addition of a drop of anisole and a drop of water. Stirred overnight at ambient temperature. The volatiles were removed in vacuo and the crude material was purified by taking up in MeOH and filtering to remove insolubles. The filtrate was concentrated in vacuo, and the resulting solid titrated with ether to give the title compound. 1H NMR (400 MHz, DMSO): 10.70 (br s, 1H), 7.17 (br m, 1H), 7.00 (s, 1H), 6.88 (s, 1H), 4.42 (d, 2H), 4.37 (s, 2H), 3.55 (m, 2H), 3.45 (m, 2H), 3.24 (s, 3H). MS (ES+): M/Z 484, 486 and 488 (M+1).

Aufarbeitung

  1. customThe volatiles were removed in vacuo
  2. customthe crude material was purified
  3. filtrationfiltering
  4. customto remove insolubles
  5. concentrationThe filtrate was concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-d80f64f82d8142f887ff464e1b22859b
Quelldatensatz
uspto-grants-2014_05
Patentnummer
US08716320B2

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