Reaktionsgleichung
C(N=C=NC[CH2:7][CH2:8][N:9]([CH2:12][CH3:13])[CH2:10][CH3:11])C.[NH2:14][C:15]1[S:16][C:17]2[C:18](=[CH:20][C:21]3[N:22]=[C:23]([NH2:27])[S:24][C:25]=3[CH:26]=2)[N:19]=1.[CH2:28]([N:30]([CH2:35][CH3:36])[CH2:31][C:32](O)=[O:33])[CH3:29].[OH2:37]>C(Cl)Cl>[CH2:28]([N:30]([CH2:31][C:32]([NH:27][C:23]1[S:24][C:25]2[C:21](=[CH:20][C:18]3[N:19]=[C:15]([NH:14][C:7](=[O:37])[CH2:8][N:9]([CH2:12][CH3:13])[CH2:10][CH3:11])[S:16][C:17]=3[CH:26]=2)[N:22]=1)=[O:33])[CH2:35][CH3:36])[CH3:29]Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
1.0 gm of ethyl-3-(3-diethylamino-propyl)-carbodiimide was added to a suspension of 555 mgm of 2,6-diamino-benzo[1,2-d:5,4-d']bisthiazole and 655 mgm of N,N-diethyl-glycine in 20 ml of methylene chloride, and the mixture was stirred overnight at room temperature. After adding water and filtering off the precipitate, the methylene chloride phase was separated, dried, concentrated and chromatographed on a dry 10 gm-silicagel column with chloroform as the mobile phase. The title compound was collected in the first fractions and converted into the dihydrochloride by treatment with ethereal hydrochloric acid.
Aufarbeitung
- filtrationfiltering off the precipitate
- customthe methylene chloride phase was separated
- customdried
- concentrationconcentrated
- customchromatographed on a dry 10 gm-silicagel column with chloroform as the mobile phase
- customThe title compound was collected in the first fractions
Quellen und Nachweise
- ORD-Eintrag
- ord-3ec3306dde864a7c99f123a38144561b
- Quelldatensatz
- uspto-grants-1982_08
- Patentnummer
- US04344946
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