Methylamine → HCID 178485071, Verbindung

HRID 1155774Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1155774
[C:1]([N:3]=[C:4](SC)[NH:5][CH2:6][CH2:7][S:8][CH2:9][C:10]1[N:14]=[C:13]([NH:15][C:16]([NH2:18])=[NH:17])[S:12][N:11]=1)#[N:2].[CH3:21][NH2:22]>C(O)C>[C:1]([N:3]=[C:4]([NH:22][CH3:21])[NH:5][CH2:6][CH2:7][S:8][CH2:9][C:10]1[N:14]=[C:13]([NH:15][C:16]([NH2:18])=[NH:17])[S:12][N:11]=1)#[N:2]

Komponenten

4

Edukt 2

HCID 6329MethylamineHCID 1785039313-[2-(3-Cyano-2-methylisothioureido)ethylthiomethyl]-5-guanidino-1,2,4-thiadiazole

Produkt 1

HCID 178485071HCID 178485071, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A suspension of 3-[2-(3-cyano-2-methylisothioureido)-ethylthiomethyl]-5-guanidino-1,2,4-thiadiazole (10 g.) in ethanol (200 ml.) was stirred and cooled to 10° with external ice cooling. Methylamine (166 g.) was passed into the suspension over 2 hours at such a rate that the temperature did not rise above 17° with external ice cooling. After 80 g. had been added, all was in solution. After 4 hours the ice bath was removed and excess methylamine was allowed to evaporate overnight. The final volume was about 120 ml. The product was filtered off, washed with a little ethanol, sucked dry and dried at 60°/0.3 m.m. Recrystallisation from aqueous ethanol (1:3 v/v) gave 3-[2-(2-cyano-3-methylguanidino)-ethylthiomethyl]-5-guanidino-1,2,4-thiadiazole, m.p. 198°-199°.

Aufarbeitung

  1. temperaturecooled to 10° with external ice cooling
  2. customdid not rise above 17° with external ice cooling
  3. additionhad been added
  4. customAfter 4 hours the ice bath was removed
  5. customto evaporate overnight
  6. filtrationThe product was filtered off
  7. washwashed with a little ethanol
  8. customsucked dry
  9. customdried at 60°/0.3 m
  10. customRecrystallisation from aqueous ethanol (1:3 v/v)

Quellen und Nachweise

ORD-Eintrag
ord-a0540596c50e469c8229b1ada68b93e4
Quelldatensatz
uspto-grants-1982_06
Patentnummer
US04332949

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