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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
ノート
印刷プレビュー

反応式

HRID 743724 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 6344Dichloromethane溶媒2 回HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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 (

出典と根拠

ORDレコード
ord-58c7fc289bf8439abe9dc5d3302e1145
出典データセット
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05556990

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート