Reacción #1135805

ord-6591d9807b084d069a922e56e41c7bab

Ecuación de reacción

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

Condiciones de reacción

Temperatura
25°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroTo the reaction mixtures
  2. 2
    Extracciónthe mixtures were extracted with ethyl acetate
  3. 3
    LavadoThe organic layers were washed with aqueous saturated sodium bicarbonate solution
  4. 4
    Secadowere dried over anhydrous sodium sulfate
  5. 5
    ConcentraciónThe resulting mixtures were concentrated under reduced pressure

Procedimiento

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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US09380782B2uspto-grants-2016_07