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Ammonium Chloride → 4-(4-Tert-butylpiperazin-1-yl)aniline

HRID 875145
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인쇄 미리보기

반응식

HRID 875145 반응식
[C:1]([N:5]1[CH2:10][CH2:9][N:8]([C:11]2[CH:16]=[CH:15][C:14]([N+:17]([O-])=O)=[CH:13][CH:12]=2)[CH2:7][CH2:6]1)([CH3:4])([CH3:3])[CH3:2].[Cl-].[NH4+]>CO.O.[Fe]>[C:1]([N:5]1[CH2:10][CH2:9][N:8]([C:11]2[CH:12]=[CH:13][C:14]([NH2:17])=[CH:15][CH:16]=2)[CH2:7][CH2:6]1)([CH3:4])([CH3:2])[CH3:3]
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참가 물질

6

반응물 2

HCID 25517Ammonium ChlorideHCID 574441581-Tert-butyl-4-(4-nitrophenyl)piperazine

생성물 1

HCID 242791824-(4-Tert-butylpiperazin-1-yl)aniline수율 89.6%

시약·촉매·용매 3

HCID 23925Iron촉매HCID 887Methanol용매HCID 962Water용매

실험 절차

To a solution of 840 mg (3.189 mmol) of 1-tert-butyl-4-(4-nitrophenyl)piperazine in 24 mL of methanol, 904 mg (16.9 mmol) of ammonium chloride dissolved in 6 mL of water and 552 mg (9.886 mmol) of iron were added. After 7 hours, the suspension was cooled and filtered. pH was adjusted to 10 through portionwise addition of Na2CO3 to the aqueous phase. Extraction with dichloromethane yielded 667 mg of the title amine.

후처리

  1. temperaturethe suspension was cooled
  2. filtrationfiltered
  3. additionpH was adjusted to 10 through portionwise addition of Na2CO3 to the aqueous phase
  4. extractionExtraction with dichloromethane

출처 및 근거

ORD 기록
ord-a65a4aefd29a4937868104240a79cb80
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08981089B2

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