反応 #1135805

ord-6591d9807b084d069a922e56e41c7bab

反応方程式

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

反応条件

温度
25°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他To the reaction mixtures
  2. 2
    抽出the mixtures were extracted with ethyl acetate
  3. 3
    洗浄The organic layers were washed with aqueous saturated sodium bicarbonate solution
  4. 4
    乾燥were dried over anhydrous sodium sulfate
  5. 5
    濃縮The resulting mixtures were concentrated under reduced pressure

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09380782B2uspto-grants-2016_07