Reaktion #1135805

ord-6591d9807b084d069a922e56e41c7bab

Reaktionsgleichung

O=C([O-])O.[Na+]
sodium bicarbonate
Cc1c(I)cccc1-n1nn[nH]c1=O
1-(2-methyl-3-iodophenyl)-1,4-dihydrotetrazole-5-one
O=C([O-])[O-].[K+].[K+]
potassium carbonate
COS(=O)(=O)OC
dimethyl sulfate
Cc1c(I)cccc1-n1nnn(C)c1=O
1-(2-methyl-3-iodophenyl)-4-methyl-1,4-dihydrotetrazole-5-one

Lösungsmittel

Reaktionsbedingungen

Temperatur
25°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeTo the reaction mixtures
  2. 2
    Extraktionthe mixtures were extracted with ethyl acetate
  3. 3
    WaschenThe organic layers were washed with aqueous saturated sodium bicarbonate solution
  4. 4
    Trocknenwere dried over anhydrous sodium sulfate
  5. 5
    EinengenThe resulting mixtures were concentrated under reduced pressure

Vorschrift

A mixture of the above-mentioned 1-(2-methyl-3-iodophenyl)-1,4-dihydrotetrazole-5-one, potassium carbonate 17.40 g, dimethyl sulfate 5.78 g and N,N-dimethylformamide 150 mL was stirred at 25° C. for one hour. To the reaction mixtures was added aqueous saturated sodium bicarbonate solution and the mixtures were extracted with ethyl acetate. The organic layers were washed with aqueous saturated sodium bicarbonate solution and were dried over anhydrous sodium sulfate. The resulting mixtures were concentrated under reduced pressure to give 1-(2-methyl-3-iodophenyl)-4-methyl-1,4-dihydrotetrazole-5-one (hereinafter, referred to as “Intermediate (PRI-P)”) 8.10 g.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09380782B2uspto-grants-2016_07