N-(3-benzhydroxypropyl)piperazine → N-[5-[3,4-di(beta-methoxyethoxy)phenyl)-2,4-pentadienoyl]-N'-(3-benzhydroxypropyl)piperazine

HRID 652970노트

반응식

HRID 652970 반응식
[CH:1]([O:14][CH2:15][CH2:16][CH2:17][N:18]1[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.COCCO[CH2:29][O:30][C:31]1[CH:32]=[C:33]([CH:44]=[CH:45][CH:46]=[CH:47][C:48](N2CCSC2=S)=[O:49])[CH:34]=[CH:35][C:36]=1[O:37][CH2:38]OCCOC>O1CCCC1>[CH3:29][O:30][CH2:31][CH2:29][O:30][C:31]1[CH:32]=[C:33]([CH:44]=[CH:45][CH:46]=[CH:47][C:48]([N:21]2[CH2:22][CH2:23][N:18]([CH2:17][CH2:16][CH2:15][O:14][CH:1]([C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[C:8]3[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=3)[CH2:19][CH2:20]2)=[O:49])[CH:34]=[CH:35][C:36]=1[O:37][CH2:38][CH2:36][O:37][CH3:38]

참가 물질

4

반응물 2

HCID 22110970N-(3-benzhydroxypropyl)piperazineHCID 54009022N-[5-[3,4-di(beta-methoxyethoxymethoxy)phenyl]2,4-pentadienoyl]thiazolidine-2-thione

생성물 1

HCID 86741623N-[5-[3,4-di(beta-methoxyethoxy)phenyl)-2,4-pentadienoyl]-N'-(3-benzhydroxypropyl)piperazine수율 160%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of 650 mg (1.2 mmol) of N-(3-benzhydroxypropyl)piperazine in dry tetrahydrofuran (5 ml) was added a solution of 966 mg (2.0 mmol) of N-[5-[3,4-di(β-methoxyethoxymethoxy)phenyl]2,4-pentadienoyl]thiazolidine-2-thione in dry tetrahydrofuran (6 ml), and the mixture was reacted at room temperature for 14 hours. The reaction mixture was concentrated by evaporation under reduced pressure, diluted with chloroform and washed, in turn, with 2N aqueous solution of sodium hydroxide and water. The organic layer was dried over anhydrous sodium sulfate and concentrated by evaporation under reduced pressure. The residue was subjected to silica gel column chromatography, eluted with 1% methanol in chloroform, to give 1.09 g (1.6 mmol) of N-[5-[3,4-di(β-methoxyethoxy)phenyl)-2,4-pentadienoyl]-N'-(3-benzhydroxypropyl)piperazine.

후처리

  1. customthe mixture was reacted at room temperature for 14 hours
  2. concentrationThe reaction mixture was concentrated by evaporation under reduced pressure
  3. additiondiluted with chloroform
  4. washwashed, in turn, with 2N aqueous solution of sodium hydroxide and water
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. concentrationconcentrated by evaporation under reduced pressure
  7. washeluted with 1% methanol in chloroform

출처 및 근거

ORD 기록
ord-277f7cbccc2349f5bf2662ecff3387d9
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04673684

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