N-(3-benzhydroxypropyl)piperazine → N-[3-[3,5-dimethoxy-4-(beta-methoxyethoxymethoxy) phenyl]-2-propenoyl]-N'-(3-benzhydroxypropyl)piperazine

HRID 652967노트

반응식

HRID 652967 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.CON1C([C:38](=[O:58])[CH:39]=[CH:40][C:41]2[CH:46]=[C:45]([O:47][CH3:48])[C:44]([O:49][CH2:50][O:51][CH2:52][CH2:53][O:54][CH3:55])=[C:43]([O:56][CH3:57])[CH:42]=2)(OCOCCOC)C(OC)SC1=S>O1CCCC1>[CH3:48][O:47][C:45]1[CH:46]=[C:41]([CH:40]=[CH:39][C:38]([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:58])[CH:42]=[C:43]([O:56][CH3:57])[C:44]=1[O:49][CH2:50][O:51][CH2:52][CH2:53][O:54][CH3:55]

참가 물질

4

반응물 2

HCID 22110970N-(3-benzhydroxypropyl)piperazineHCID 867416223,5-Dimethoxy-4-(beta-methoxyethoxymethoxy) (3,5-dimethoxy-4(beta-methoxyethoxymethoxy) phenyl-2-propenoyl]thiazolidine-2-thione

생성물 1

HCID 53774023N-[3-[3,5-dimethoxy-4-(beta-methoxyethoxymethoxy) phenyl]-2-propenoyl]-N'-(3-benzhydroxypropyl)piperazine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of 160 mg (0.52 mmol) of N-(3-benzhydroxypropyl) piperazine in dry tetrahydrofuran (5 ml) was added a solution of 206 mg (0.5 mmol) of N-[3-(3,5-dimethoxy-4-(β-methoxyethoxymethoxy) (3,5-dimethoxy-4(β-methoxyethoxymethoxy) phenyl-2-propenoyl]thiazolidine-2-thione in dry tetrahydrofuran, and the mixture was allowed to react at room temperature overnitht. 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 chloroform - methanol (50 : 1), to give 270 mg (0.45 mmol) of N-[3-[3,5-dimethoxy-4-(β-methoxyethoxymethoxy) phenyl]-2-propenoyl]-N'-(3-benzhydroxypropyl)piperazine.

후처리

  1. customto react at room temperature overnitht
  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 chloroform - methanol (50 : 1)

출처 및 근거

ORD 기록
ord-5db78b2a04c8442b8377ced29509adb1
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04673684

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