Dimethylcarbamoyl Chloride → 2-Chloro-4-Isopropylamino-6-(2-[Dimethylcarbamylthio]ethylamino)-s-Triazine

HRID 2398052Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2398052
[Na].C[O-].[Na+].[Cl:5][C:6]1[N:11]=[C:10]([NH:12][CH:13]([CH3:15])[CH3:14])[N:9]=[C:8]([NH:16][CH2:17][CH2:18][SH:19])[N:7]=1.[CH3:20][N:21]([CH3:25])[C:22](Cl)=[O:23]>CCOCC.CC(C)=O.CO>[Cl:5][C:6]1[N:11]=[C:10]([NH:12][CH:13]([CH3:15])[CH3:14])[N:9]=[C:8]([NH:16][CH2:17][CH2:18][S:19][C:22](=[O:23])[N:21]([CH3:25])[CH3:20])[N:7]=1

Komponenten

7

Edukt 4

HCID 6598Dimethylcarbamoyl ChlorideHCID 5360545SodiumHCID 10942334Sodium MethoxideHCID 214345132-Chloro-4-isopropylamino-6-(2-mercaptoethylamino)-s-triazine

Produkt 1

HCID 214345482-Chloro-4-Isopropylamino-6-(2-[Dimethylcarbamylthio]ethylamino)-s-Triazine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 21584533Acetone diethyletherLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A 0.46-g sample of sodium was added to 50 ml methanol in small pieces. To the resulting sodium methoxide solution was added 5 g of 2-chloro-4-isopropylamino-6-(2-mercaptoethylamino)-s-triazine, followed by 2.16 g dimethylcarbamyl chloride at 0° C. The reaction mixture was heated at 80° C. for 4 hours, cooled, filtered and evaporated under reduced pressure to give a yellow oil. The yellow oil was dissolved in 1:1 ether/acetone and filtered. The filtrate was evaporated to give the product as an oil. The elemental analysis on the product is tabulated in Table I.

Aufarbeitung

  1. temperaturecooled
  2. filtrationfiltered
  3. customevaporated under reduced pressure
  4. customto give a yellow oil
  5. filtrationfiltered
  6. customThe filtrate was evaporated

Quellen und Nachweise

ORD-Eintrag
ord-2727647c427f4caaa32af7e24ba1f0f0
Quelldatensatz
uspto-grants-1977_05
Patentnummer
US04024141

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