反应 #1135805

ord-6591d9807b084d069a922e56e41c7bab

反应方程式

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

反应条件

温度
25°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他To the reaction mixtures
  2. 2
    萃取the mixtures were extracted with ethyl acetate
  3. 3
    洗涤The organic layers were washed with aqueous saturated sodium bicarbonate solution
  4. 4
    干燥were dried over anhydrous sodium sulfate
  5. 5
    浓缩The resulting mixtures were concentrated under reduced pressure

实验过程

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.

来源

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