Sodium Hydroxide → 3-[Bis(4-methoxybenzyl)amino]-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-5-phenyl-2-pyrazinecarboxamide

HRID 915042노트

반응식

HRID 915042 반응식
[CH3:1][O:2][C:3]1[CH:43]=[CH:42][C:6]([CH2:7][N:8]([CH2:33][C:34]2[CH:39]=[CH:38][C:37]([O:40][CH3:41])=[CH:36][CH:35]=2)[C:9]2[C:10]([C:31]#[N:32])=[N:11][C:12]([C:21]3[CH:26]=[CH:25][C:24](=[O:27])[N:23]([CH:28]([CH3:30])[CH3:29])[N:22]=3)=[C:13]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[N:14]=2)=[CH:5][CH:4]=1.[OH-:44].[Na+]>O1CCOCC1>[CH3:41][O:40][C:37]1[CH:36]=[CH:35][C:34]([CH2:33][N:8]([CH2:7][C:6]2[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:43][CH:42]=2)[C:9]2[C:10]([C:31]([NH2:32])=[O:44])=[N:11][C:12]([C:21]3[CH:26]=[CH:25][C:24](=[O:27])[N:23]([CH:28]([CH3:30])[CH3:29])[N:22]=3)=[C:13]([C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=3)[N:14]=2)=[CH:39][CH:38]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 693319503-[Bis(4-methoxybenzyl)amino]-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-5-phenyl-2-pyrazinecarbonitrile

생성물 1

HCID 693314613-[Bis(4-methoxybenzyl)amino]-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-5-phenyl-2-pyrazinecarboxamide

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A suspension of 3-[bis(4-methoxybenzyl)amino]-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-5-phenyl-2-pyrazinecarbonitrile (3.00 g) in a mixture of 2N aq. NaOH (30 ml) and dioxane (21 ml) was refluxed for 36 hours. After cooling, the mixture was extracted with EtOAc, dried over MgSO4, concentrated under reduced pressure and purified by column chromatography on silica gel eluting with a mixture of n-hexane and EtOAc (20:80 v/v) to give a solid. The solid was crystallized from a mixture of n-hexane and acetone to give 3-[bis(4-methoxybenzyl)amino]-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-5-phenyl-2-pyrazinecarboxamide (2.56 g).

후처리

  1. temperaturewas refluxed for 36 hours
  2. temperatureAfter cooling
  3. extractionthe mixture was extracted with EtOAc
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated under reduced pressure
  6. custompurified by column chromatography on silica gel eluting with a mixture of n-hexane and EtOAc (20:80 v/v)
  7. customto give a solid
  8. customThe solid was crystallized from a mixture of n-hexane and acetone

출처 및 근거

ORD 기록
ord-0c5045c4dea24c65b65cb1c317af4a01
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07265120B2

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