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1,2-Dichloroethane → Ethyl 4-[3-hydroxy-3-(4-naphth-2-yl-phenyl)piperidin-1-ylcarbonyl]-3-hydroxy-3-ethoxycarbonylbutanoate

HRID 743724
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HRID 743724 반응식
[OH:1][C:2]1([C:8]2[CH:13]=[CH:12][C:11]([C:14]3[CH:23]=[CH:22][C:21]4[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=4)[CH:15]=3)=[CH:10][CH:9]=2)[CH2:7][CH2:6][CH2:5][NH:4][CH2:3]1.[OH:24][C:25]([C:36]([O:38][CH2:39][CH3:40])=[O:37])([CH2:30][C:31]([O:33][CH2:34][CH3:35])=[O:32])[CH2:26][C:27](O)=[O:28].C(Cl)CCl.ON1C2C=CC=CC=2N=N1.C(N(CC)CC)C>C1COCC1.C(Cl)Cl.C(OCC)(=O)C>[OH:1][C:2]1([C:8]2[CH:9]=[CH:10][C:11]([C:14]3[CH:23]=[CH:22][C:21]4[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=4)[CH:15]=3)=[CH:12][CH:13]=2)[CH2:7][CH2:6][CH2:5][N:4]([C:27]([CH2:26][C:25]([OH:24])([C:36]([O:38][CH2:39][CH3:40])=[O:37])[CH2:30][C:31]([O:33][CH2:34][CH3:35])=[O:32])=[O:28])[CH2:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 111,2-DichloroethaneHCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 153840823-Hydroxy-3-(4-naphth-2-ylphenyl)piperidineHCID 15384083Diethyl Citrate

생성물 1

HCID 19424723Ethyl 4-[3-hydroxy-3-(4-naphth-2-yl-phenyl)piperidin-1-ylcarbonyl]-3-hydroxy-3-ethoxycarbonylbutanoate
수율 75%

시약·촉매·용매 3

HCID 6344Dichloromethane용매2회HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

3-Hydroxy-3-(4-naphth-2-ylphenyl)piperidine (Preparation 7, 1.24 g, 4.09 mmol), 3-hydroxy-3, 4-bis(ethoxycarbonyl)butanoic acid (Preparation 1, 1.01 g, 4.09 mmol), EDC, (0.785 g, 4.09 mmol), 1-hydroxybenzotriazole (HOBT, 0.055 g, 2.05 mmol) and triethylamine (570 μL, 8.18 mmol) in THF or methylene chloride (150 mL) is stirred under argon overnight. The reaction mixture is diluted with CH2Cl2 or ethyl acetate and washed with water or 5% aqueous hydrochloric acid, saturated aqueous sodium bicarbonate, and brine. The organic layer is then dried over MgSO4 or Na2SO4, filtered and concentrated. The crude product is purified by flash chromatography (using 60% ethyl acetate in hexane in this instance) to yield the diester intermediate, ethyl 4-[3-hydroxy-3-(4-naphth-2-yl-phenyl)piperidin-1-ylcarbonyl]-3-hydroxy-3-ethoxycarbonylbutanoate (1.63 g, 75%) as a foam solid.

후처리

  1. washwashed with water or 5% aqueous hydrochloric acid, saturated aqueous sodium bicarbonate, and brine
  2. dry with materialThe organic layer is then dried over MgSO4 or Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe crude product is purified by flash chromatography (

출처 및 근거

ORD 기록
ord-58c7fc289bf8439abe9dc5d3302e1145
출처 데이터셋
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05556990

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