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Oxalyl chloride → HCID 59255047、化合物

HRID 639548
ノート
印刷プレビュー

反応式

HRID 639548 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:13]([OH:15])=O)[C:5](=[O:12])[N:6]([CH:9]([CH3:11])[CH3:10])[C:7]=1[CH3:8].C(Cl)(=O)C(Cl)=O.[NH2:22][CH2:23][CH:24]1[CH2:29][CH2:28][N:27]([C:30]([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31])[CH2:26][CH2:25]1.C(N(CC)C(C)C)(C)C>ClCCl.CN(C)C=O>[Cl:1][C:2]1[CH:3]=[C:4]([C:13]([NH:22][CH2:23][CH:24]2[CH2:29][CH2:28][N:27]([C:30]([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31])[CH2:26][CH2:25]2)=[O:15])[C:5](=[O:12])[N:6]([CH:9]([CH3:10])[CH3:11])[C:7]=1[CH3:8]
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 65578Oxalyl chlorideHCID 81531DiisopropylethylamineHCID 7368171-Boc-4-(aminomethyl)piperidineHCID 59255058HCID 59255058、化合物

生成物 1

HCID 59255047HCID 59255047、化合物収率 99%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide
溶媒
HCID 6344Dichloromethane溶媒

実験手順

To a solution of 5-chloro-1-isopropyl-6-methyl-2-oxo-1,2-dihydropyridine-3-carboxylic acid as prepared in Example 1(7) (2.66 g, 11.6 mmol) in dichloromethane (30 mL) were added oxalyl chloride (4.41 g, 34.8 mmol) and a drop of N,N-dimethylformamide at room temperature, and the mixture was stirred at room temperature for 2 h. The solvent and excess amounts of oxalyl chloride were removed in vacuo. The residue was dissolved in dichloromethane (80 mL). To the resulting solution were added tert-butyl 4-(aminomethyl)piperidine-1-carboxylate (3.72 g, 17.4 mmol, prepared according to Carceller, Elena et al., J. Med. Chem., 1996, 39, 487), N,N-diisopropylethylamine (2.25 g, 17.4 mmol) at room temperature, and the mixture was stirred at room temperature for 18 h. Then, the mixture was quenched with saturated sodium hydrogencarbonate aqueous solution (100 mL), and extracted with dichloromethane (100 mL×4). The combined organic layers were dried over magnesium sulfate and concentrated in vacuo. The residue was chromatographed on a column of silica gel eluting with n-hexane/ethyl acetate (v/v=1/1) to give 5.27 g (99%) of the title compound as a white solid.

後処理

  1. customThe solvent and excess amounts of oxalyl chloride were removed in vacuo
  2. dissolutionThe residue was dissolved in dichloromethane (80 mL)
  3. customThen, the mixture was quenched with saturated sodium hydrogencarbonate aqueous solution (100 mL)
  4. extractionextracted with dichloromethane (100 mL×4)
  5. dry with materialThe combined organic layers were dried over magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe residue was chromatographed on a column of silica gel eluting with n-hexane/ethyl acetate (v/v=1/1)

出典と根拠

ORDレコード
ord-fed3a04627d644c4bd9b01a9ef78e2fe
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07691881B2

反応ノート

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