2-Methyl-2-thiopseudourea sulfate → HCID 131715810, Verbindung

HRID 2291591Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2291591
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][C:8](=[O:10])[N:7]([CH2:11][C:12]([N:14]3[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]3)=[O:13])[C:6]=2[CH:20]=1.[S:21]([OH:25])([OH:24])(=[O:23])=[O:22].CS[C:28](=[NH:30])[NH2:29]>CN(C)C=O.O>[S:21]([OH:25])([OH:24])(=[O:23])=[O:22].[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][C:8](=[O:10])[N:7]([CH2:11][C:12]([N:14]3[CH2:15][CH2:16][N:17]([C:28](=[NH:29])[NH2:30])[CH2:18][CH2:19]3)=[O:13])[C:6]=2[CH:20]=1.[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][C:8](=[O:10])[N:7]([CH2:11][C:12]([N:14]3[CH2:15][CH2:16][N:17]([C:28](=[NH:29])[NH2:30])[CH2:18][CH2:19]3)=[O:13])[C:6]=2[CH:20]=1

Komponenten

5

Edukt 2

HCID 752702-Methyl-2-thiopseudourea sulfateHCID 169502Rhc 3281

Produkt 1

HCID 131715810HCID 131715810, VerbindungAusbeute 67,8 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

To a solution of 5-chloro-3-[(1-piperazinyl)carbonylmethyl]-2-benzothiazolinone (3.0 g) in a mixture of N,N-dimethylformamide (30 ml) and water (5 ml) was added S-methylisothiourea sulfate (4.0 g). The mixture was stirred for 8 hours at 80° C. and then cooled. The precipitates formed were filtered and recrystallized from water (100 ml) to give 5-chloro-3-[(4-amidino-1-piperazinyl)carbonylmethyl]-2-benzothiazolinone hemisulfate (2.63 g).

Aufarbeitung

  1. temperaturecooled
  2. customThe precipitates formed
  3. filtrationwere filtered
  4. customrecrystallized from water (100 ml)

Quellen und Nachweise

ORD-Eintrag
ord-28c4aec52cfe4d03b881f09d53698562
Quelldatensatz
uspto-grants-1989_01
Patentnummer
US04797399

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