Potassium Acetate → 2-[4-[(4-Chlorophenyl)cyanomethyl]-3-methoxyphenyl]2,3,4,5-tetrahydro-3,5-dioxo-1,2,4-triazine-6-carbonitrile

HRID 1710027

反応式

HRID 1710027 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:30]#[N:31])[C:9]2[CH:14]=[CH:13][C:12]([NH:15][N:16]=[C:17]([C:26]#[N:27])[C:18]([NH:20][C:21](=O)[O:22]CC)=[O:19])=[CH:11][C:10]=2[O:28][CH3:29])=[CH:4][CH:3]=1.C([O-])(=O)C.[K+]>C(O)(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:30]#[N:31])[C:9]2[CH:14]=[CH:13][C:12]([N:15]3[C:21](=[O:22])[NH:20][C:18](=[O:19])[C:17]([C:26]#[N:27])=[N:16]3)=[CH:11][C:10]=2[O:28][CH3:29])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 517044Potassium AcetateHCID 86742407Ethyl [2-[[4-[(4-chlorophenyl)cyanomethyl]-3-methoxyphenyl]hydrazono]-2-cyanoacetyl]carbamate

生成物 1

HCID 230351972-[4-[(4-Chlorophenyl)cyanomethyl]-3-methoxyphenyl]2,3,4,5-tetrahydro-3,5-dioxo-1,2,4-triazine-6-carbonitrile

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

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.

後処理

  1. temperatureat reflux temperature
  2. customThe reaction mixture is evaporated in vacuo
  3. stirringThe residue is stirred in water
  4. filtrationThe product is filtered off
  5. dissolutiondissolved in trichloromethane
  6. customThe organic layer is dried
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue is purified by column chromatography over silica gel using
  10. additiona mixture of trichloromethane and methanol (90:10 by volume) as eluent
  11. customThe pure fractions are collected
  12. customthe eluent is evaporated in vacuo

出典と根拠

ORDレコード
ord-1d780a640ab74f9c862f9151602cf3cc
出典データセット
uspto-grants-1990_08
特許番号
US04952570

関連ノート

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