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Methylhydrazine → HCID 69447489、化合物

HRID 1593010
ノート
印刷プレビュー

反応式

HRID 1593010 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14](=O)[CH2:15][C:16](=O)[CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH3:26][NH:27][NH2:28]>CO>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]2[N:27]([CH3:26])[N:28]=[C:16]([CH2:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH:15]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6061MethylhydrazineHCID 18187492Tert-butyl 4-(3-oxo-4-phenylbutanoyl)piperidine-1-carboxylate

生成物 1

HCID 69447489HCID 69447489、化合物収率 26.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

4-(3-Oxo-4-phenyl-butyryl)-piperidine-1-carboxylic acid tert-butyl ester (0.118 g) was dissolved in MeOH (4 mL) and added to a refluxing solution of methyl hydrazine (0.019 g) in methanol (2 mL). After 45 minutes at reflux the reaction mixture was cooled to room temperature and solvents evaporated under reduced pressure to give the crude product as a clear oil which was purified by column chromatography on silica using Et2O as eluent to give 4-(5-benzyl-2-methyl-2H-pyrazol-3-yl)-piperidine-1-carboxylic acid tert-butyl ester (0.032 g) as a clear oil; NMR (CDCl3): 1.46 (s, 9H), 1.46-1.54 (m, 2H), 1.82 (br d, 2H), 2.64 (tt, 1H), 2.78 (br t, 2H), 3.77 (s, 3H), 3.90 (s, 2H), 4.18 (br d, 2H), 5.72 (s, 1H), 7.16-7.29 (m, 5H); MS: 356 (MH+).

後処理

  1. temperatureAfter 45 minutes at reflux the reaction mixture
  2. customsolvents evaporated under reduced pressure
  3. customto give the crude product as a clear oil which
  4. customwas purified by column chromatography on silica

出典と根拠

ORDレコード
ord-7c1a6497bf8d4425a5780a0df8b15ff5
出典データセット
uspto-grants-2007_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07294636B2

反応ノート

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