반응 #1135805

ord-6591d9807b084d069a922e56e41c7bab

반응 방정식

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

반응 조건

온도
25°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타To the reaction mixtures
  2. 2
    추출the mixtures were extracted with ethyl acetate
  3. 3
    세척The organic layers were washed with aqueous saturated sodium bicarbonate solution
  4. 4
    건조were dried over anhydrous sodium sulfate
  5. 5
    농축The resulting mixtures were concentrated under reduced pressure

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09380782B2uspto-grants-2016_07