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Sodium Hydroxide → HCID 21448529、化合物

HRID 596854
ノート
印刷プレビュー

反応式

HRID 596854 の反応式
O=C1CNCCN1.[CH2:8]([N:10]([CH2:26][CH3:27])[CH:11]([N:13]1[CH2:18][CH2:17][NH:16][C:15](=O)[CH:14]1[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH3:12])[CH3:9].O1CCOCC1.[OH-].[Na+]>O.CCOCC>[CH2:26]([N:10]([CH2:8][CH3:9])[CH:11]([N:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH:14]1[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH3:12])[CH3:27]
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 14798Sodium Hydroxide2 回HCID 312751,4-DioxaneHCID 231360Piperazin-2-one2 回HCID 214485351-Diethylamino ethyl-2-phenyl-3-keto piperazine

生成物 1

HCID 21448529HCID 21448529、化合物収率 77%

試薬・触媒・溶媒 2

HCID 962Water
溶媒
2 回
HCID 3283Diethyl Ether溶媒

実験手順

89 g. of the keto piperazine prepared as described hereinabove under (a), are dissolved in 200 cc. of absolute dioxane. The solution is added to a suspension of 20 g. of lithium aluminum hydride LiAlH4 in 800 cc. of absolute ether while exposing the mixture to vibration. After addition of the keto piperazine solution is completed, the reaction mixture is boiled under reflux for 6 hours. Thereafter it is decomposed by successive treatment with 21 cc. of 15 % sodium hydroxide solution, 21 cc. of water, 63 cc. of 15 % sodium hydroxide solution, and 42 cc. of water. The decomposed reaction mixture is filtered, the solvent is removed by distillation, and the residue is distilled in a vacuum. 65 g. of a light yellow oil of the boiling point 114°-117° C./0.05 mm. Hg are obtained. This oil corresponds to the above given compound. The yield is 77 % of the theoretical yield.

後処理

  1. dissolutionare dissolved in 200 cc
  2. additionThe solution is added to a suspension of 20 g
  3. temperatureunder reflux for 6 hours
  4. customThe decomposed reaction mixture
  5. filtrationis filtered
  6. customthe solvent is removed by distillation
  7. distillationthe residue is distilled in a vacuum
  8. customof a light yellow oil of the boiling point 114°-117° C./0.05 mm. Hg are obtained

出典と根拠

ORDレコード
ord-748f04f311ae4e9d834b456f17142940
出典データセット
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04012389

反応ノート

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