反応 #63831

反応方程式

ethyl [2-[[4-[(4-chlorophenyl)cyanomethyl]-3-methoxyphenyl]hydrazono]-2-cyanoacetyl]carbamate

potassium acetate

→

2-[4-[(4-chlorophenyl)cyanomethyl]-3-methoxyphenyl]-2,3,4,5-tetrahydro-3,5-dioxo-1,2,4-triazine-6-carbonitrile

溶媒

acetic acid

反応条件

後処理

1. 1
   温度at reflux temperature
2. 2
   その他The reaction mixture is evaporated in vacuo
3. 3
   workup.STIRRINGThe residue is stirred in water
4. 4
   ろ過The product is filtered off
5. 5
   workup.DISSOLUTIONdissolved in trichloromethane
6. 6
   その他The organic layer is dried
7. 7
   ろ過filtered
8. 8
   その他evaporated
9. 9
   その他The residue is purified by column chromatography over silica gel using
10. 10
    workup.ADDITIONa mixture of trichloromethane and methanol (90:10 by volume) as eluent
11. 11
    その他The pure fractions are collected
12. 12
    その他the eluent is evaporated in vacuo

実験手順

A mixture of 8.3 parts of ethyl [2-[[4-[(4-chlorophenyl)cyanomethyl]-3-methoxyphenyl]hydrazono]-2-cyanoacetyl]carbamate, 1.77 parts of anhydrous potassium acetate and 100 parts of acetic acid is stirred for 2 hours at reflux temperature. The reaction mixture is evaporated in vacuo. The residue is stirred in water. The product is filtered off and dissolved in trichloromethane. The organic layer is dried, filtered and evaporated. The residue is purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (90:10 by volume) as eluent. The pure fractions are collected and the eluent is evaporated in vacuo, yielding 2-[4-[(4-chlorophenyl)cyanomethyl]-3-methoxyphenyl]-2,3,4,5-tetrahydro-3,5-dioxo-1,2,4-triazine-6-carbonitrile.

出典