Triethylamine → 1-[5-(3,4,5-Trimethoxyphenyl)-2,4-pentadienoyl]-4-(methylaminocarbonylmethyl)-piperazine

HRID 542179

반응식

HRID 542179 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:13]=[CH:14][CH:15]=[CH:16][C:17]([N:19]2[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]2)=[O:18])[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10].C(N(CC)CC)C.[CH3:32][NH:33][C:34](=[O:37])[CH2:35]Cl>C1(C)C=CC=CC=1.C1(C)C=CC=CC=1.C(Cl)(Cl)Cl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:13]=[CH:14][CH:15]=[CH:16][C:17]([N:19]2[CH2:20][CH2:21][N:22]([CH2:35][C:34]([NH:33][CH3:32])=[O:37])[CH2:23][CH2:24]2)=[O:18])[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10]

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 667732-chloro-N-methylacetamideHCID 539540541-[5-(3,4,5-Trimethoxyphenyl)-2,4-pentadienoyl]-piperazine

생성물 1

HCID 544790041-[5-(3,4,5-Trimethoxyphenyl)-2,4-pentadienoyl]-4-(methylaminocarbonylmethyl)-piperazine수율 71.7%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 22987606Toluene trichloromethane용매

실험 절차

To a solution of 302 mg of 1-[5-(3,4,5-trimethoxyphenyl)-2,4-pentadienoyl]-piperazine in dry toluene (12 ml) were added in an atmosphere of argon 1.3 ml of triethylamine and subsequently a solution of 254 mg of N-methylchloroacetamide in dry toluene-chloroform (1:1, 2 ml). The mixture was refluxed for 8 hours. To the reaction mixture was added water, and extraction was made with methylene chloride. The organic layer was concentrated under reduced pressure, and the residue thus obtained was chromatographed on silica gel column. There was obtained 263 mg of 1-[5-(3,4,5-trimethoxyphenyl)-2,4-pentadienoyl]-4-(methylaminocarbonylmethyl)-piperazine. Spectrophotometric data of the product support the structure of the formula (V) shown below. ##STR5##

후처리

  1. temperatureThe mixture was refluxed for 8 hours
  2. additionTo the reaction mixture was added
  3. extractionwater, and extraction
  4. concentrationThe organic layer was concentrated under reduced pressure
  5. customthe residue thus obtained
  6. customwas chromatographed on silica gel column

출처 및 근거

ORD 기록
ord-253f5fbbf2084f0f95c1c0e20c2f9ce3
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04656172

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