StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Sodium Carbonate → HCID 21259081, Verbindung

HRID 635508
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 635508
NC1N=C2C(NC=N2)=C(Cl)N=1.[CH:12]([NH:14][C:15]1[N:23]=[C:22]2[C:18]([NH:19][CH:20]=[N:21]2)=[C:17]([Cl:24])[N:16]=1)=[O:13].P(Cl)(Cl)(Cl)=O.N1[C:39](=[O:40])[C:38]2NC=NC=2N=C1N.C(=O)([O-])[O-].[Na+].[Na+]>O.ClCCCl.CN(C)C=O>[C:39]([OH:40])(=[O:13])[CH3:38].[CH:12]([NH:14][C:15]1[N:23]=[C:22]2[C:18]([NH:19][CH:20]=[N:21]2)=[C:17]([Cl:24])[N:16]=1)=[O:13]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 10340Sodium CarbonateHCID 24813Phosphorus oxychlorideHCID 53603492-Amino-6-chloropurine2×HCID 109283082-Formylamino-6-chloropurineHCID 135398634Guanine

Produkt 1

HCID 21259081HCID 21259081, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel

3
HCID 111,2-DichloroethaneLösungsmittelHCID 962WaterLösungsmittel2×HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

The 2-amino-6-chloropurine having an acicular or irregular-shaped crystal form can be prepared by hydrolyzing 2-formylamino-6-chloropurine or a salt thereof in water in the presence of an acid or an alkali, followed by neutralizing the resulting reaction mixture. For example, the 2-amino-6-chloropurine having an acicular or irregular-shaped crystal form can be produced by a conventional method as disclosed in JP-6-157530. Specifically, dimethylformamide, phosphorus oxychloride and guanine are added to 1,2-dichloroethane, and the mixture is stirred with heating. After cooling, the reaction mixture is added to water, to which sodium carbonate is added to adjust the pH of the mixture to 4. Then, the aqueous layer is separated therefrom, which is then neutralized by adding sodium hydroxide thereto. The precipitated crystal of 2-dimethylaminomethyleneamino-6-chloropurine is filtered off and added to an aqueous solution of acetic acid. The solution is stirred with heating to precipitate crystals. The precipitated crystals are filtered off and washed with water to give crystals of 2-formylamino-6-chloropurine acetate. The crystals of 2-formylamino-6-chloropurine acetate are then dissolved in an aqueous solution of a metal hydroxide such as sodium hydroxide with stirring. The solution is neutralized with hydrochloric acid, acetic acid or sulfuric acid to precipitate crystals. The precipitated crystals are filtered off to obtain acicular or irregular-shaped white crystals of 2-amino-6-chloropurine.

Aufarbeitung

  1. customthe resulting reaction mixture
  2. temperaturewith heating
  3. temperatureAfter cooling
  4. additionis added
  5. customThen, the aqueous layer is separated
  6. additionby adding sodium hydroxide
  7. filtrationThe precipitated crystal of 2-dimethylaminomethyleneamino-6-chloropurine is filtered off
  8. additionadded to an aqueous solution of acetic acid
  9. stirringThe solution is stirred
  10. temperaturewith heating
  11. customto precipitate crystals
  12. filtrationThe precipitated crystals are filtered off
  13. washwashed with water

Quellen und Nachweise

ORD-Eintrag
ord-e4078dcd600c407dafeeb7e6daf3a7b6
Quelldatensatz
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06187921B1

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion