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1,4-Dioxane hydrochloride → N-{4-[2-(4-hydrazinocarbonylmethylphenyl)ethyl]phenyl}acetamide hydrochloride

HRID 1465434
ノート
印刷プレビュー

反応式

HRID 1465434 の反応式
O1CCOCC1.[ClH:7].[C:8]([NH:11][C:12]1[CH:17]=[CH:16][C:15]([CH2:18][CH2:19][C:20]2[CH:25]=[CH:24][C:23]([CH2:26][C:27]([NH:29][NH:30]C(OC(C)(C)C)=O)=[O:28])=[CH:22][CH:21]=2)=[CH:14][CH:13]=1)(=[O:10])[CH3:9]>>[ClH:7].[NH:29]([C:27]([CH2:26][C:23]1[CH:22]=[CH:21][C:20]([CH2:19][CH2:18][C:15]2[CH:14]=[CH:13][C:12]([NH:11][C:8](=[O:10])[CH3:9])=[CH:17][CH:16]=2)=[CH:25][CH:24]=1)=[O:28])[NH2:30]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 204431481,4-Dioxane hydrochlorideHCID 67030250Tert-butyl 2-({4-[(4-acetamidophenyl)ethyl]phenyl}acetyl)hydrazinecarboxylate

生成物 1

HCID 67030104N-{4-[2-(4-hydrazinocarbonylmethylphenyl)ethyl]phenyl}acetamide hydrochloride収率 98%

実験手順

4M-Hydrogen chloride dioxane solution (1 ml, 4 mmol) was added to tert-butyl 2-({4-[(4-acetamidophenyl)ethyl]phenyl}acetyl)hydrazinecarboxylate (23 mg, 0.056 mmol), and the mixture was stirred at room temperature for 15 mins. The reaction mixture was concentrated under reduced pressure, dichloromethane was added, and the mixture was concentrated again, and hydrogen chloride gas was removed. The precipitate was collected by filtration, washed with diethyl ether and dried under reduced pressure to give the title compound (18 mg, yield 98%) as a slightly yellow solid.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure, dichloromethane
  2. additionwas added
  3. concentrationthe mixture was concentrated again
  4. customhydrogen chloride gas was removed
  5. filtrationThe precipitate was collected by filtration
  6. washwashed with diethyl ether
  7. customdried under reduced pressure

出典と根拠

ORDレコード
ord-cab499f9c9944612ae025fd8380c79e1
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08999989B2

反応ノート

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