Sodium Hydroxide → HCID 178458744, Verbindung

HRID 442491Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 442491
[CH3:1][N:2]([CH3:11])[C:3]1[N:8]=[C:7]([OH:9])[CH:6]=[C:5]([OH:10])[N:4]=1.[OH-].[Na+].[CH2:14](OS(C1C=CC(C)=CC=1)(=O)=O)[CH2:15][CH3:16]>C(O)(=O)C>[CH3:1][N:2]([CH3:11])[C:3]1[N:4]=[C:5]([O:10][CH2:14][CH2:15][CH3:16])[CH:6]=[C:7]([OH:9])[N:8]=1

Komponenten

5

Edukt 3

HCID 14798Sodium Hydroxide2×HCID 69035Propyl p-toluenesulfonateHCID 178483102HCID 178483102, Verbindung

Produkt 1

HCID 178458744HCID 178458744, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

124 g (0.8 mol) of 2-dimethylamino-4,6-dihydroxy-pyrimidine are stirred with 800 cc of sodium hydroxide solution 1N at 60° for 1 hour. 171 g (0.8 mol) of p-toluene-sulphonic acid-n-propyl ester are added dropwise at 90° over the course of 1 hour and the pH is kept at 8-8.5 by the dropwise addition of sodium hydroxide solution 1N. The mixture is stirred at 90° for 16 hours, cooled to 5°, neutralized with glacial acetic acid and allowed to stand at room temperature for 6 hours. The precipitated crystals are subsequently filtered by suction, washed with water, dissolved in approximately 700 cc of chloroform, dried over sodium sulphate and evaporated to dryness in a vacuum. The residue is decomposed with 500 cc of petroleum ether, filtered by suction and recrystallized from benzene, washed with petroleum ether and dried at 60° in a high vacuum. M.P.: 194°-195°

Aufarbeitung

  1. temperaturecooled to 5°
  2. waitto stand at room temperature for 6 hours
  3. filtrationThe precipitated crystals are subsequently filtered by suction
  4. washwashed with water
  5. dissolutiondissolved in approximately 700 cc of chloroform
  6. dry with materialdried over sodium sulphate
  7. customevaporated to dryness in a vacuum
  8. filtrationfiltered by suction
  9. customrecrystallized from benzene
  10. washwashed with petroleum ether
  11. customdried at 60° in a high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-631dca2a6e0744229a2d9a4e4c972f9e
Quelldatensatz
uspto-grants-1977_08
Patentnummer
US04045561

Notizen zur Reaktion

Wird geladen…