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Hydroxylamine → tert-butyl 4-(N-hydroxyamidino)-piperazine-1-carboxylate

HRID 888178
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HRID 888178 반응식
[C:1]([N:3]1[CH2:8][CH2:7][N:6]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:5][CH2:4]1)#[N:2].[NH2:16][OH:17]>C(O)C>[OH:17][NH:16][C:1](=[NH:2])[N:3]1[CH2:4][CH2:5][N:6]([C:9]([O:11][C:12]([CH3:14])([CH3:13])[CH3:15])=[O:10])[CH2:7][CH2:8]1
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참가 물질

4

반응물 2

HCID 787HydroxylamineHCID 14068968tert-Butyl 4-cyanopiperazine-1-carboxylate

생성물 1

HCID 178452346tert-butyl 4-(N-hydroxyamidino)-piperazine-1-carboxylate수율 80.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of tert-butyl 4-cyanopiperazine-1-carboxylate (15 g, 76 mmol) in ethanol (150 mL) was added hydroxylamine (50% aqueous solution, 6.2 mL, 92 mmol) and the reaction mixture was stirred at RT for 6 hours. The solvent was evaporated under vacuum and the solid obtained was triturated with hexane (100 mL) and filtered to obtain 15 g (80%) of the title compound as a solid. TLC-Chloroform/methanol (9/1): Rf=0.15.

후처리

  1. customThe solvent was evaporated under vacuum
  2. customthe solid obtained
  3. customwas triturated with hexane (100 mL)
  4. filtrationfiltered

출처 및 근거

ORD 기록
ord-ec7ddd5bec6f4099bb5f3dc07cecc918
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08247437B2

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