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

HRID 35553노트

반응식

HRID 35553 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 230351972-[4-[(4-Chlorophenyl)cyanomethyl]-3-methoxyphenyl]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 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.

후처리

  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

출처 및 근거

ORD 기록
ord-e1c5ca6a3c794839854921db2ff067ac
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04767760

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