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Hydrochloric Acid → N-hydroxy-2-[(3,4-dimethoxyphenyl)thio]-3-(3-phenylpropyl-1-yl)-1-cyclopentenecarboxamide

HRID 1107130
ノート
印刷プレビュー

反応式

HRID 1107130 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([S:11][C:12]2[C:16](=[CH:17][CH2:18][CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[CH2:15][CH2:14][C:13]=2[C:26]([OH:28])=O)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].C(Cl)(=O)C(Cl)=O.C[Si](C)(C)[O:37][NH2:38].Cl>ClCCl>[OH:37][NH:38][C:26]([C:13]1[CH2:14][CH2:15][C:16](=[CH:17][CH2:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:12]=1[S:11][C:5]1[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=1)=[O:28]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 65578Oxalyl chlorideHCID 2734666O-(Trimethylsilyl)hydroxylamineHCID 699076212-[(3,4-Dimethoxyphenyl)thio]-3-(3-phenylpropyl-1-yl)-1-cyclopentenecarboxylic acid

生成物 1

HCID 86755387N-hydroxy-2-[(3,4-dimethoxyphenyl)thio]-3-(3-phenylpropyl-1-yl)-1-cyclopentenecarboxamide

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

To a solution of 2-[(3,4-dimethoxyphenyl)thio]-3-(3-phenylpropyl-1-yl)-1-cyclopentenecarboxylic acid (0.6 g, 1.5 mmol) in dichloromethane (20 mL) is added 2 M oxalyl chloride (1.5 mL, 3 mmol). The mixture is stirred at room temperature for 15 minutes. The solvent is removed in vacuo and the residue is dissolved in dichloromethane and O-(trimethylsilyl)hydroxylamine (0.3 mL, 3 mmol) is added. The mixture is stirred at room temperature for 30 minutes. The mixture is poured into 5% HCl and is extracted with dichloromethane. The organic layer is washed with water and is dried over MgSO4. The solvent is removed in vacuo and the residue is chromatographed on silica gel (100% ethyl acetate). The product is dissolved in the minimum amount of ethyl acetate and the solution is diluted to the cloudy point with hexane to precipitate N-hydroxy-2-[(3,4-dimethoxyphenyl)thio]-3-(3-phenylpropyl-1-yl)-1-cyclopentenecarboxamide on standing at room temperature overnight (0.1 g, 16%): m.p. 44-6° C. Anal. (C23H27NO4S.1/4H2O) C,H,N: 1H-NMR (300 MHz, CDCl3) δ (TMS) 1.42-1.78 (m, 5H), 1.90-2.08 (m, 1H), 2.38-2.50 (m, 2H), 2.59-2.78 (m, 3H), 3.82 (s, 3H), 3.90 (s, 3H), 6.72-6.79 (d, 1H), 6.88-6.98 (m, 2H), 6.98-7.10 (d, 2H), 7.10-7.30 (m, 3H), 9.02 (s, 1H); MS (Ion Spray) m/e 413 (M+H)+.

後処理

  1. customThe solvent is removed in vacuo
  2. dissolutionthe residue is dissolved in dichloromethane
  3. stirringThe mixture is stirred at room temperature for 30 minutes
  4. extractionis extracted with dichloromethane
  5. washThe organic layer is washed with water
  6. dry with materialis dried over MgSO4
  7. customThe solvent is removed in vacuo
  8. customthe residue is chromatographed on silica gel (100% ethyl acetate)
  9. dissolutionThe product is dissolved in the minimum amount of ethyl acetate
  10. additionthe solution is diluted to the cloudy point with hexane
  11. customto precipitate N-hydroxy-2-[(3,4-dimethoxyphenyl)thio]-3-(3-phenylpropyl-1-yl)-1-cyclopentenecarboxamide
  12. waiton standing at room temperature overnight

出典と根拠

ORDレコード
ord-d2d931b5633343cea97471c0eae4d837
出典データセット
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06057369

反応ノート

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