Реакция #1135805

ord-6591d9807b084d069a922e56e41c7bab

Уравнение реакции

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

Растворители

Условия реакции

Температура
25°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеTo the reaction mixtures
  2. 2
    Экстракцияthe mixtures were extracted with ethyl acetate
  3. 3
    ПромывкаThe organic layers were washed with aqueous saturated sodium bicarbonate solution
  4. 4
    Сушкаwere dried over anhydrous sodium sulfate
  5. 5
    КонцентрированиеThe resulting mixtures were concentrated under reduced pressure

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09380782B2uspto-grants-2016_07