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

HRID 355361ノート

反応式

HRID 355361 の反応式
C([O:3][C:4](=O)[NH:5][C:6](=[O:30])[C:7](=[N:10][NH:11][C:12]1[CH:17]=[C:16]([Cl:18])[C:15]([CH:19]([C:22]2[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][CH:23]=2)[C:20]#[N:21])=[C:14]([Cl:29])[CH:13]=1)[C:8]#[N:9])C.C([O-])(=O)C.[K+]>C(O)(=O)C>[Cl:29][C:14]1[CH:13]=[C:12]([N:11]2[C:4](=[O:3])[NH:5][C:6](=[O:30])[C:7]([C:8]#[N:9])=[N:10]2)[CH:17]=[C:16]([Cl:18])[C:15]=1[CH:19]([C:22]1[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][CH:23]=1)[C:20]#[N:21]

参加物

4

反応物 2

HCID 517044Potassium AcetateHCID 131720911HCID 131720911、化合物2 回

生成物 1

HCID 189421712-[3,5-Dichloro-4-[(4-chlorophenyl)cyanomethyl]phenyl]-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 7.8 parts of ethyl[2-[[3,5-dichloro-4-[(4-chlorophenyl)cyanomethyl]phenyl]hydrazono]-2-cyanoacetyl]carbamate (intermediate 3), 1.98 parts of anhydrous potassium acetate and 120 parts of acetic acid is stirred and heated under reflux for 3 hours. The reaction mixture is concentrated to a volume of 30 parts. Water is added until the product is precipitated. It is sucked off, washed with water and dissolved in trichloromethane. The remaining water is separated and the organic phase is dried, filtered and evaporated, yielding 2-[3,5-dichloro-4-[(4-chlorophenyl)cyanomethyl]phenyl]-2,3,4,5-tetrahydro-3,5-dioxo-1,2,4-triazine-6-carbonitrile (intermediate 4).

後処理

  1. temperatureheated
  2. temperatureunder reflux for 3 hours
  3. concentrationThe reaction mixture is concentrated to a volume of 30 parts
  4. additionWater is added until the product
  5. customis precipitated
  6. washwashed with water
  7. dissolutiondissolved in trichloromethane
  8. customThe remaining water is separated
  9. customthe organic phase is dried
  10. filtrationfiltered
  11. customevaporated

出典と根拠

ORDレコード
ord-4f04aa85a2f24b8aad9342e20a01596f
出典データセット
uspto-grants-1998_11
特許番号
US05830893

反応ノート

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