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

HRID 1465434
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인쇄 미리보기

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HRID 1465434 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cab499f9c9944612ae025fd8380c79e1
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08999989B2

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