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Acetic Acid → HCID 69333276, 화합물

HRID 915037
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HRID 915037 반응식
[NH2:1][C:2]1[C:3]([C:25]#[N:26])=[N:4][C:5]([C:15]2[CH:20]=[CH:19][C:18](=[O:21])[N:17]([CH:22]([CH3:24])[CH3:23])[N:16]=2)=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=2)[N:7]=1.CC(O)=[O:29].O.C([O-])(O)=O.[Na+]>Br.CCOC(C)=O>[NH2:1][C:2]1[C:3]([C:25]([NH2:26])=[O:29])=[N:4][C:5]([C:15]2[CH:20]=[CH:19][C:18](=[O:21])[N:17]([CH:22]([CH3:24])[CH3:23])[N:16]=2)=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=2)[N:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 962WaterHCID 516892Sodium BicarbonateHCID 69332723HCID 69332723, 화합물

생성물 1

HCID 69333276HCID 69333276, 화합물

시약·촉매·용매 2

HCID 260Hydrogen Bromide용매
HCID 8857
Ethyl Acetate
용매

실험 절차

A solution of 3-amino-5-(4-fluorophenyl)-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-2-pyrazinecarbonitrile (30 mg) in 28% hydrogen bromide solution of AcOH (2 ml) was stirred at 25° C. for 3 hours. Water, aq. NaHCO3 and EtOAc were added to the reaction mixture. The organic layer was separated, and dried over MgSO4. The solvent was removed in vacuo. The residue was purified by silica gel column chromatography eluted with a mixture of CHCl3 and MeOH. The fractions were concentrated in vacuo to obtain 3-amino-5-(4-fluorophenyl)-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-2-pyrazinecarboxamide (30 g) as white powder.

후처리

  1. customThe organic layer was separated
  2. dry with materialdried over MgSO4
  3. customThe solvent was removed in vacuo
  4. customThe residue was purified by silica gel column chromatography
  5. washeluted with a mixture of CHCl3 and MeOH
  6. concentrationThe fractions were concentrated in vacuo

출처 및 근거

ORD 기록
ord-423610b02c314db096c9c813aefed529
출처 데이터셋
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07265120B2

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