HCID 21273587, Verbindung → HCID 178429718, Verbindung

HRID 846909Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 846909
[SH:1][C:2]1[N:7]2[N:8]=[C:9]([C:11](OC)=[O:12])[N:10]=[C:6]2[N:5]=[C:4]([CH3:15])[CH:3]=1.[H-].C([Al+]CC(C)C)C(C)C.CCCCCC>O1CCCC1>[SH:1][C:2]1[N:7]2[N:8]=[C:9]([CH2:11][OH:12])[N:10]=[C:6]2[N:5]=[C:4]([CH3:15])[CH:3]=1

Komponenten

4

Edukt 2

HCID 21273587HCID 21273587, VerbindungHCID 178499048HCID 178499048, Verbindung

Produkt 1

HCID 178429718HCID 178429718, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

2.24 g of methyl 7-mercapto-5-methyl-s-triazolo[1,5-a]-pyrimidine-2-carboxylate were suspended in 350 ml of tetrahydrofuran and treated at 2° within 15 minutes with 40 ml of a 1M diisobutylaluminium hydride/hexane solution. The reaction mixture was stirred at 2° for 10 minutes and subsequently treated with ice. The reaction mixture was concentrated extensively, the residue was taken up in 30 ml of water, and the solution was acidified to pH 1.2 with concentrated hydrochloric acid. The solid was collected by filtration and dried in a high vacuum. There was obtained 7-mercapto-5-methyl-s-tria-zolo[1,5-a]pyrimidine-2-methanol of melting point 233° (dec.).

Aufarbeitung

  1. additionsubsequently treated with ice
  2. concentrationThe reaction mixture was concentrated extensively
  3. filtrationThe solid was collected by filtration
  4. customdried in a high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-b45379e3a06f4054b076533b8fd9cceb
Quelldatensatz
uspto-grants-1992_08
Patentnummer
US05138066

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