Toluene → S-[(6-Chloro-5-oxo-5H-thiazolo[3,2-a]pyrimidin-7-yl)methyl] O,O-dimethyl phosphorodithioate

HRID 1075294Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1075294
[Cl:1][C:2]1[C:7](=[O:8])[N:6]2[CH:9]=[CH:10][S:11][C:5]2=[N:4][C:3]=1[CH2:12]Cl.C1(C)C=CC=CC=1.[P:21]([S-:27])(=[S:26])([O:24][CH3:25])[O:22][CH3:23].[NH4+]>CO>[P:21]([S:27][CH2:12][C:3]1[N:4]=[C:5]2[S:11][CH:10]=[CH:9][N:6]2[C:7](=[O:8])[C:2]=1[Cl:1])(=[S:26])([O:24][CH3:25])[O:22][CH3:23]

Komponenten

5

Edukt 3

HCID 1140TolueneHCID 6451175Ammonium O,O-dimethyl dithiophosphateHCID 132329226-Chloro-7-(chloromethyl)-5H-[1,3]thiazolo[3,2-a]pyrimidin-5-one

Produkt 1

HCID 13232940S-[(6-Chloro-5-oxo-5H-thiazolo[3,2-a]pyrimidin-7-yl)methyl] O,O-dimethyl phosphorodithioate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

The compound of EXAMPLE 2 (7 g) and 100 ml of toluene was stirred and heated to 70°. To this mixture was added, dropwise, a solution of 14 g ammonium dimethyl phosphorodithioate in 200 ml methanol. The resulting mixture was kept at 70° for 6 hours, then the methanol was distilled off. Toluene (400 ml) was added, and the mixture was washed with water, separated, dried and evaporated under reduced pressure. The solid which remained was washed with toluene and filtered. The solid, m.p. 125°-130°, weighed 2.5 g.

Aufarbeitung

  1. temperatureheated to 70°
  2. additionTo this mixture was added
  3. distillationthe methanol was distilled off
  4. additionToluene (400 ml) was added
  5. washthe mixture was washed with water
  6. customseparated
  7. customdried
  8. customevaporated under reduced pressure
  9. washThe solid which remained was washed with toluene
  10. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-40ccea17e8c74c6ab6bb42fa09a6de52
Quelldatensatz
uspto-grants-1983_07
Patentnummer
US04395551

Notizen zur Reaktion

Wird geladen…