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Hydrochloric Acid → HCID 178427282, Verbindung

HRID 483246
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 483246
[NH2:1][C:2]1[C:6]([NH:7][CH2:8][CH2:9][S:10][CH2:11][C:12]2[S:13][C:14]([CH2:18][N:19]([CH3:21])[CH3:20])=[C:15]([CH3:17])[CH:16]=2)=[N:5]S(=O)[N:3]=1.[ClH:23]>CO>[ClH:23].[ClH:23].[ClH:23].[CH3:21][N:19]([CH2:18][C:14]1[S:13][C:12]([CH2:11][S:10][CH2:9][CH2:8][NH:7][C:6](=[NH:5])[C:2](=[NH:1])[NH2:3])=[CH:16][C:15]=1[CH3:17])[CH3:20]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 23312524HCID 23312524, Verbindung

Produkt 1

HCID 178427282HCID 178427282, VerbindungAusbeute 80 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A stirred solution of 3-amino-4-{2-[(5-dimethylaminomethyl-4-methyl-2-thienyl)methylthio]ethylamino}-1,2,5-thiadiazole 1-oxide (17.9 g, 50.0 mmoles) [prepared according to the general procedure described in published United Kingdom Patent Application No. 2,067,987] in 500 mL of methanol was treated with 33.3 mL of concentrated HCl. After stirring for 3 hours, the reaction mixture was concentrated and excess water was removed by azeotropic concentration with absolute ethanol to give an almost colorless crystalline residue. The residue was triturated with 200 mL of absolute ethanol at 0° C., filtered and dried to give 16.9 g (80%) of the title compound, m.p. 206°-220° C. (dec.). Recrystallization from 50% methanol-ethyl acetate gave a product having m.p. 210°-221° C. (dec.).

Aufarbeitung

  1. concentrationthe reaction mixture was concentrated
  2. customexcess water was removed by azeotropic concentration with absolute ethanol
  3. customto give an almost colorless crystalline residue
  4. customThe residue was triturated with 200 mL of absolute ethanol at 0° C.
  5. filtrationfiltered
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-0b3f1b4ce6304297bc87950b4b3c85a9
Quelldatensatz
uspto-grants-1986_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04578471

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