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Pyridine → 4-(4-Chloro-phenyl)-3-methoxycarbonylmethyl-piperazine-1-carboxylic acid tert-butyl ester

HRID 557084
ノート
印刷プレビュー

反応式

HRID 557084 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5](B(O)O)=[CH:4][CH:3]=1.[C:11]([O:15][C:16]([N:18]1[CH2:23][CH2:22][NH:21][CH:20]([CH2:24][C:25]([O:27][CH3:28])=[O:26])[CH2:19]1)=[O:17])([CH3:14])([CH3:13])[CH3:12].N1C=CC=CC=1>ClCCl.C([O-])(=O)C.[Cu+2].C([O-])(=O)C>[C:11]([O:15][C:16]([N:18]1[CH2:23][CH2:22][N:21]([C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=2)[CH:20]([CH2:24][C:25]([O:27][CH3:28])=[O:26])[CH2:19]1)=[O:17])([CH3:14])([CH3:13])[CH3:12]
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 3

HCID 1049PyridineHCID 742994-Chlorophenylboronic acidHCID 2756816Methyl 4-Boc-piperazine-2-acetate

生成物 1

HCID 667586684-(4-Chloro-phenyl)-3-methoxycarbonylmethyl-piperazine-1-carboxylic acid tert-butyl ester

試薬・触媒・溶媒 2

HCID 8895Cupric acetate触媒HCID 6344
Dichloromethane
溶媒

実験手順

4-Chlorophenyl boronic acid (1.08 g, 6.97 mmol) and 3-methoxycarbonylmethyl-piperazine-1-carboxylic acid tert-butyl ester (0.9 g, 3.48 mmol) were dissolved in dichloromethane. To this mixture was added copper acetate (0.63 g, 3.48 mmol), 4 Å molecular sieves and pyridine (0.56 mL, 6.97 mmol) and the reaction mixture was stirred at room temperature for 72 h. The reaction mixture was concentrated in vacuo and dissolved in ethyl acetate, filtered through celite and concentrated. The crude product was purified using gradient elution from hexane/ethyl acetate (5%) to hexane/ethyl acetate (20%). ESI-MS m/z: 369 (M+1), UV retention time: 2.97 min.

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. dissolutiondissolved in ethyl acetate
  3. filtrationfiltered through celite
  4. concentrationconcentrated
  5. customThe crude product was purified
  6. washelution from hexane/ethyl acetate (5%) to hexane/ethyl acetate (20%)

出典と根拠

ORDレコード
ord-5061cc2b504e4a00b6ade102f85b0527
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08058287B2

反応ノート

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