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Water → 2,6-dichloro-N-[2-hydroxy-4-(4-methyl-6-oxo-1,4,5,6-tetrahydro-pyridazin-3-yl)-phenyl]-nicotinamide

HRID 1619977
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HRID 1619977 반응식
[Cl:1][C:2]1[N:10]=[C:9]([Cl:11])[CH:8]=[CH:7][C:3]=1[C:4](Cl)=[O:5].[NH2:12][C:13]1[CH:18]=[CH:17][C:16]([C:19]2[CH:20]([CH3:26])[CH2:21][C:22](=[O:25])[NH:23][N:24]=2)=[CH:15][C:14]=1[OH:27].C(=O)([O-])[O-].[K+].[K+].O>CN(C=O)C>[Cl:1][C:2]1[N:10]=[C:9]([Cl:11])[CH:8]=[CH:7][C:3]=1[C:4]([NH:12][C:13]1[CH:18]=[CH:17][C:16]([C:19]2[CH:20]([CH3:26])[CH2:21][C:22](=[O:25])[NH:23][N:24]=2)=[CH:15][C:14]=1[OH:27])=[O:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 122639842,6-Dichlorpyridine-3-carbonyl chlorideHCID 179934936-(4-amino-3-hydroxy-phenyl)-5-methyl-4,5-dihydro-2H-pyridazin-3-one

생성물 1

HCID 866890692,6-dichloro-N-[2-hydroxy-4-(4-methyl-6-oxo-1,4,5,6-tetrahydro-pyridazin-3-yl)-phenyl]-nicotinamide

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매
2회

실험 절차

A solution of 8.5 g (0.0405 mol) 2,6-dichloronicotinoyl chloride in 20 ml DMF is slowly added dropwise to a suspension of 8.8 g (0.04 mol) 6-(4-amino-3-hydroxy-phenyl)-5-methyl-4,5-dihydro-2H-pyridazin-3-one, 6.9 g (0.05 mol) potassium carbonate and 50 ml DMF and it is then stirred overnight. The reaction mixture is mixed with water, then the aqueous supernatant is decanted off, the residue is washed with water again, filtered off and then purified through silica gel (eluant: ethylene chloride/ethanol).

후처리

  1. customthe aqueous supernatant is decanted off
  2. washthe residue is washed with water again
  3. filtrationfiltered off
  4. custompurified through silica gel (eluant: ethylene chloride/ethanol)

출처 및 근거

ORD 기록
ord-ad1ec46c20504092aa258f4206056195
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08772323B2

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