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HCID 123928403, 화합물 → HCID 123244203, 화합물

HRID 1509228
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HRID 1509228 반응식
[C:1]([O:5][C:6](=[O:37])[NH:7][C:8]1([C:12]2[CH:17]=[CH:16][C:15]([C:18]3[C:23]([C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=4)=[CH:22][C:21]([N+:30]([O-])=O)=[C:20]([CH2:33][N+:34]([O-])=O)[N:19]=3)=[CH:14][CH:13]=2)[CH2:11][CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2]>CCO.[Ni]>[C:1]([O:5][C:6](=[O:37])[NH:7][C:8]1([C:12]2[CH:13]=[CH:14][C:15]([C:18]3[C:23]([C:24]4[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=4)=[CH:22][C:21]([NH2:30])=[C:20]([CH2:33][NH2:34])[N:19]=3)=[CH:16][CH:17]=2)[CH2:9][CH2:10][CH2:11]1)([CH3:4])([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 123928403HCID 123928403, 화합물

생성물 1

HCID 123244203HCID 123244203, 화합물

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

To a solution of tert-butyl(1-(4-(5-nitro-6-(nitromethyl)-3-phenylpyridin-2-yl)phenyl)cyclobutyl)carbamate (74 mg, 0.15 mmol) in EtOH (50 mL) was added Raney Nickel (17 mg, 0.15 mmol). The resulting mixture was purged with nitrogen and with H2 and then stirred under H2 (1.5 bars) overnight at room temperature. The black mixture was filtered through celite, rinsed few times with EtOH (making sure that the cake remained wet at all times), dried over Na2SO4 and concentrated to dryness under reduced pressure. The resulting residue was used directly without purification.

후처리

  1. customThe resulting mixture was purged with nitrogen and with H2
  2. filtrationThe black mixture was filtered through celite
  3. washrinsed few times with EtOH (
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated to dryness under reduced pressure
  6. customThe resulting residue was used directly without purification

출처 및 근거

ORD 기록
ord-b52d5dc8d80d4325a0faa179d6019f44
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09221838B2

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