Methanol → 4-amino-N-(2-amino-6-methoxy-pyrimidin-4-yl)-benzenesulfonamide

HRID 378285Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 378285
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12]2[CH:17]=[C:16](Cl)[N:15]=[C:14]([NH2:19])[N:13]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.[CH3:20][OH:21]>[Na]>[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12]2[CH:17]=[C:16]([O:21][CH3:20])[N:15]=[C:14]([NH2:19])[N:13]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 887MethanolHCID 107329394-amino-N-(2-amino-6-chloro-pyrimidin-4-yl)-benzenesulfonamide

Produkt 1

HCID 193535384-amino-N-(2-amino-6-methoxy-pyrimidin-4-yl)-benzenesulfonamideAusbeute 94 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 5360545SodiumLösungsmittel

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

0.27 g (0.0009 mol) of 4-amino-N-(2-amino-6-chloro-pyrimidin-4-yl)-benzenesulfonamide was dissolved in a solution of 0.23 g of sodium in 20 ml of methanol and stirred in an autoclave at 150° C. for 9 hours. The solvent was distilled off, the residue was added to water and the pH value was adjusted to 4-5 with 1N HCl. The precipitate which thereby separated was filtered off under suction, washed with water and dried. The crystals obtained were triturated in 20 ml of methanol, again filtered off and dried in a high vacuum. There was obtained 0.25 g (94%) of 4-amino-N-(2-amino-6-methoxy-pyrimidin-4-yl)-benzenesulfonamide as beige crystals; m.p.: >250° C. (dec.).

Aufarbeitung

  1. distillationThe solvent was distilled off
  2. additionthe residue was added to water
  3. customThe precipitate which thereby separated
  4. filtrationwas filtered off under suction
  5. washwashed with water
  6. customdried
  7. customThe crystals obtained
  8. customwere triturated in 20 ml of methanol
  9. filtrationagain filtered off
  10. customdried in a high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-cc7321af0d8043c7bdbd2e5918423a78
Quelldatensatz
uspto-grants-2000_02
Patentnummer
US06030976

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