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 355361노트

반응식

HRID 355361 반응식
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]

참가 물질

4

반응물 2

HCID 517044Potassium AcetateHCID 131720911HCID 131720911, 화합물2회

생성물 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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-4f04aa85a2f24b8aad9342e20a01596f
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05830893

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