Réaction #1135805

ord-6591d9807b084d069a922e56e41c7bab

Équation de réaction

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

Conditions de réaction

Température
25°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    AutreTo the reaction mixtures
  2. 2
    Extractionthe mixtures were extracted with ethyl acetate
  3. 3
    LavageThe organic layers were washed with aqueous saturated sodium bicarbonate solution
  4. 4
    Séchagewere dried over anhydrous sodium sulfate
  5. 5
    ConcentrationThe resulting mixtures were concentrated under reduced pressure

Mode opératoire

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.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US09380782B2uspto-grants-2016_07