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Sodium Hydroxide → HCID 21448529, 화합물

HRID 596854
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HRID 596854 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 14798Sodium Hydroxide2회HCID 312751,4-DioxaneHCID 231360Piperazin-2-one2회HCID 214485351-Diethylamino ethyl-2-phenyl-3-keto piperazine

생성물 1

HCID 21448529HCID 21448529, 화합물수율 77%

시약·촉매·용매 2

HCID 962Water
용매
2회
HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-748f04f311ae4e9d834b456f17142940
출처 데이터셋
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04012389

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