Potassium Carbonate → tert-butyl 4-[4-[(E)-hydroxyiminomethyl]phenyl]piperazine-1-carboxylate

HRID 1744119ノート

反応式

HRID 1744119 の反応式
[CH:1]([C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH2:10]2)=[CH:5][CH:4]=1)=O.C([O-])([O-])=O.[K+].[K+].Cl.[NH2:29][OH:30]>CCO.O>[OH:30]/[N:29]=[CH:1]/[C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH2:10]2)=[CH:5][CH:4]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 2795509Tert-butyl 4-(4-formylphenyl)piperazine-1-carboxylate

生成物 1

HCID 22236181tert-butyl 4-[4-[(E)-hydroxyiminomethyl]phenyl]piperazine-1-carboxylate

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a suspension of tert-butyl 4-(4-formylphenyl)piperazine-1-carboxylate (3.89 g, 13.41 mmol, prepared as described in Example 10) and K2CO3 (1.02 g, 7.38 mmol) in EtOH (50 mL) was added hydroxylamine hydrochloride (1.4 g, 20.1 mmol) in water (saturated, approx. 2 mL) and the reaction mixture stirred overnight. The reaction was filtered, concentrated in vacuo, water was added and the product filtered to afford tert-butyl 4-{4-[(E)-(hydroxyimino)methyl]phenyl}piperazine-1-carboxylate.

後処理

  1. filtrationThe reaction was filtered
  2. concentrationconcentrated in vacuo, water
  3. additionwas added
  4. filtrationthe product filtered

出典と根拠

ORDレコード
ord-a24cf33f4a6c4e0ca12136bc80f2f7ef
出典データセット
uspto-grants-2006_03
特許番号
US07012075B2

反応ノート

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