Water → 6-(1-Isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-3-[(4-methoxybenzyl)amino]-5-phenyl-2-pyrazinecarbonitrile

HRID 915022노트

반응식

HRID 915022 반응식
[CH:1]([N:4]1[C:9](=[O:10])[CH:8]=[CH:7][C:6]([C:11]2[N:12]=[C:13]([C:25]#[N:26])[C:14](C#N)=[N:15][C:16]=2[C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[N:5]1)([CH3:3])[CH3:2].[CH3:27][O:28][C:29]1[CH:36]=[CH:35][C:32]([CH2:33][NH2:34])=[CH:31][CH:30]=1.O.CCCCCC>CC(N(C)C)=O.CCOC(C)=O>[CH:1]([N:4]1[C:9](=[O:10])[CH:8]=[CH:7][C:6]([C:11]2[N:12]=[C:13]([C:25]#[N:26])[C:14]([NH:34][CH2:33][C:32]3[CH:35]=[CH:36][C:29]([O:28][CH3:27])=[CH:30][CH:31]=3)=[N:15][C:16]=2[C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)=[N:5]1)([CH3:2])[CH3:3]

참가 물질

7

반응물 4

HCID 962WaterHCID 8058HexaneHCID 754524-MethoxybenzylamineHCID 693333355-(1-Isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-6-phenyl-2,3-pyrazinedicarbonitrile

생성물 1

HCID 693318746-(1-Isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-3-[(4-methoxybenzyl)amino]-5-phenyl-2-pyrazinecarbonitrile

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 31374Dimethylacetamide용매

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온도
82.5 °C

실험 절차

A mixture of 5-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-6-phenyl-2,3-pyrazinedicarbonitrile (343 mg) and (4-methoxybenzyl)amine (0.137 ml) in DMA (1 ml) was heated at 80-85° C. for 25 hours. After addition of water, a precipitate was collected by filtration, dissolved in CHCl3, dried over MgSO4 and concentrated under reduced pressure to give a residue. The residue was subjected to column chromatography on silica gel eluting with a mixture of n-hexane and EtOAc (60:40 v/v) to give 6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-3-[(4-methoxybenzyl)amino]-5-phenyl-2-pyrazinecarbonitrile as an amorphous solid (227 mg).

후처리

  1. filtrationa precipitate was collected by filtration
  2. dissolutiondissolved in CHCl3
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated under reduced pressure
  5. customto give a residue

출처 및 근거

ORD 기록
ord-4ffd0b7469d2473e9604a7375a4fda4d
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07265120B2

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