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Hexane → (1R)-cyclopropanecarboxylic acid {2-[1-(3-ethoxy-4-methoxy-phenyl)-3-hydroxy-propyl]-3-oxo-2,3-dihydro-1H-isoindol-4-yl}-amide

HRID 658144
ノート
印刷プレビュー

反応式

HRID 658144 の反応式
[NH2:1][C@@H:2]([C:6]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[C:8]([O:14][CH2:15][CH3:16])[CH:7]=1)[CH2:3][CH2:4][OH:5].C[O:18][C:19](=O)[C:20]1[C:25]([NH:26][C:27]([CH:29]2[CH2:31][CH2:30]2)=[O:28])=[CH:24][CH:23]=[CH:22][C:21]=1[CH2:32]Br.C(N(CC)CC)C.CCCCCC>CN(C=O)C.CCOCC>[CH2:15]([O:14][C:8]1[CH:7]=[C:6]([C@H:2]([N:1]2[C:19](=[O:18])[C:20]3[C:21](=[CH:22][CH:23]=[CH:24][C:25]=3[NH:26][C:27]([CH:29]3[CH2:31][CH2:30]3)=[O:28])[CH2:32]2)[CH2:3][CH2:4][OH:5])[CH:11]=[CH:10][C:9]=1[O:12][CH3:13])[CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8058HexaneHCID 8471TriethylamineHCID 669203212-Bromomethyl-6-(cyclopropanecarbonyl-amino)-benzoic acid methyl esterHCID 67175570(3R)-3-amino-3-(3-ethoxy-4-methoxyphenyl)propan-1-ol

生成物 1

HCID 9845251(1R)-cyclopropanecarboxylic acid {2-[1-(3-ethoxy-4-methoxy-phenyl)-3-hydroxy-propyl]-3-oxo-2,3-dihydro-1H-isoindol-4-yl}-amide収率 64%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

実験手順

A solution of (3R)-3-amino-3-(3-ethoxy-4-methoxy-phenyl)-propan-1-ol (1.1 g, 4.9 mmol), 2-bromomethyl-6-(cyclopropanecarbonyl-amino)-benzoic acid methyl ester (1.5 g, 4.8 mmol) and triethylamine (0.75 mL, 5.4 mmol) in DMF (10 mL) was heated at 100° C. for 18 h. The solvent was removed in vacuo. The residue was extracted with ethyl acetate (50 mL) and water (50 mL). The organic layer was washed with HCl (1N, 50 mL), brine (50 mL), and dried over MgSO4. The solvent was removed in vacuo to give an oil. The oil was stirred in ether (5 mL) and hexane (5 mL) to give a suspension. The suspension was filtered to give (1R)-cyclopropanecarboxylic acid {2-[1-(3-ethoxy-4-methoxy-phenyl)-3-hydroxy-propyl]-3-oxo-2,3-dihydro-1H-isoindol-4-yl}-amide as a white solid (1.3 g, 64% yield): mp, 103-105° C.; 1H NMR (CDCl3) δ 0.86-0.93 (m, 2H, CH2), 1.08-1.12 (m, 2H, CH2), 1.44 (t, J=7 Hz, 3H, CH3), 1.64-1.73 (m, 1H, CH), 2.11-2.32 (m, 2H, CH2), 3.37 (dd, J=4, 9 Hz, 1H, OH), 3.50-3.59 (m, 1H, CHH), 3.74-3.79 (m, 2H, NCHH, CHH), 3.80 (s, 3H, CH3), 4.06 (q, J=7 Hz, 2H, CH2), 4.16 (d, J=18 Hz, 1H, NCHH), 6.65 (dd, J=4, 11 Hz, 1H, NCH), 6.83-6.99 (m, 4H, Ar), 7.44 (t, J=8 Hz, 1H, Ar), 8.45 (d, J=8 Hz, 1H, Ar), 10.52 (s, 1H, NH); 13C NMR (CDCl3) δ 8.35, 14.77, 16.22, 33.85, 46.23, 50.52, 55.98, 58.59, 64.55, 111.36, 112.99, 116.77, 116.99, 117.83, 119.77, 130.73, 133.37, 138.05, 141.49, 148.62, 149.25, 170.33, 172.76; Anal Calcd for C24H28N2O5: C, 67.91; H, 6.65; N, 6.60. Found: C, 67.92; H, 6.67; N, 6.37.

後処理

  1. customThe solvent was removed in vacuo
  2. extractionThe residue was extracted with ethyl acetate (50 mL) and water (50 mL)
  3. washThe organic layer was washed with HCl (1N, 50 mL), brine (50 mL)
  4. dry with materialdried over MgSO4
  5. customThe solvent was removed in vacuo
  6. customto give an oil
  7. filtrationThe suspension was filtered

出典と根拠

ORDレコード
ord-9ee1b29fcfed49228b359c30b978ed0b
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08076369B2

反応ノート

読み込み中…

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