Hydrogen Bromide → HCID 19705067, Verbindung

HRID 1081594

Reaktionsgleichung

Reaktionsgleichung von HRID 1081594
C(O[CH2:9][C:10]1[N:15]=[C:14]([NH2:16])[N:13]=[C:12]([NH2:17])[C:11]=1[C:18]1[CH:23]=[CH:22][C:21]([Cl:24])=[CH:20][C:19]=1[Cl:25])C1C=CC=CC=1.[BrH:26]>C(O)(=O)C>[NH2:16][C:14]1[N:13]=[C:12]([NH2:17])[C:11]([C:18]2[CH:23]=[CH:22][C:21]([Cl:24])=[CH:20][C:19]=2[Cl:25])=[C:10]([CH2:9][Br:26])[N:15]=1

Komponenten

4

Edukt 2

HCID 260Hydrogen BromideHCID 115236576-Benzyloxymethyl-2,4-diamino-5-(2,4-dichlorophenyl)pyrimidine

Produkt 1

HCID 19705067HCID 19705067, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

2,4-Diamino-6-benzyloxymethyl-5-(2,4-dichlorophenyl)pyrimidine (Example 26) (6.5 g) was dissolved in a 47% solution of hydrobromic acid in acetic acid (75 ml) and the mixture stirred and heated at 100° C. for 6 hours. After standing at room temperature overnight the dihydrobromide salt was filtered off, washed with ether and dried in vacuo, 6 g. To a stirred solution of the dihydrobromide salt (0.43 g) in dimethylsulphoxide (4 ml) was added dropwise a solution of sodium bicarbonate (0.84 g) in water (10 ml). After 30 minutes the precipitate was filtered off washed with water then ether and dried in vacuo, 0.26 g, mp.>270° C. (decomposes).

Aufarbeitung

  1. filtrationthe dihydrobromide salt was filtered off
  2. washwashed with ether
  3. customdried in vacuo, 6 g
  4. additionTo a stirred solution of the dihydrobromide salt (0.43 g) in dimethylsulphoxide (4 ml) was added dropwise a solution of sodium bicarbonate (0.84 g) in water (10 ml)
  5. filtrationAfter 30 minutes the precipitate was filtered off
  6. washwashed with water
  7. dry with materialether and dried in vacuo, 0.26 g, mp.>270° C. (decomposes)

Quellen und Nachweise

ORD-Eintrag
ord-ac6f1b8cd2cd4ac199eefa730bcb7891
Quelldatensatz
uspto-grants-1996_12
Patentnummer
US05587380

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