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Hydrazine → Benzyl 4-(6-methyl-3-oxo-2,3,4,5-tetrahydropyridazine-4-yl)piperidine-1-carboxylate

HRID 1664780
ノート
印刷プレビュー

反応式

HRID 1664780 の反応式
[NH2:1][NH2:2].C([O:5][C:6]([CH:8]([CH:13]1[CH2:18][CH2:17][N:16]([C:19]([O:21][CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=[O:20])[CH2:15][CH2:14]1)[CH2:9][C:10](=O)[CH3:11])=O)C>C(O)(=O)C>[CH3:11][C:10]1[CH2:9][CH:8]([CH:13]2[CH2:18][CH2:17][N:16]([C:19]([O:21][CH2:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)=[O:20])[CH2:15][CH2:14]2)[C:6](=[O:5])[NH:1][N:2]=1
参加物反応条件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 9321HydrazineHCID 67438602Benzyl 4-[1-(ethoxycarbonyl)-3-oxobutyl]piperidine-1-carboxylate

生成物 1

HCID 67438628Benzyl 4-(6-methyl-3-oxo-2,3,4,5-tetrahydropyridazine-4-yl)piperidine-1-carboxylate

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
50 °C

実験手順

Hydrazine (4.72 mL, 148.7 mmol) was added to a solution of benzyl 4-[1-(ethoxycarbonyl)-3-oxobutyl]piperidine-1-carboxylate (2.69 g, 7.44 mmol) in acetic acid (110 mL). The reaction mixture was heated at 50° C. After 1 h, the reaction mixture was concentrated. The residue was diluted with dichloromethane, neutralized by saturated aqueous sodium bicarbonate. The mixture was extracted with dichloromethane (3×), and the combined organic extracts were dried over magnesium sulfate and concentrated to give the title compound. MS 330.2 (M+1).

後処理

  1. concentrationthe reaction mixture was concentrated
  2. additionThe residue was diluted with dichloromethane
  3. extractionThe mixture was extracted with dichloromethane (3×)
  4. dry with materialthe combined organic extracts were dried over magnesium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-c29e158e98c84ad5aa6f438638272007
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08039460B2

反応ノート

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