Acetic Acid → 6-[2-(2,6-dichloro-pyridin-3-yl)-benzoxazol-6-yl]-5-methyl-4,5-dihydro-2H-pyridazin-3-one

HRID 1619978노트

반응식

HRID 1619978 반응식
[Cl:1][C:2]1[N:25]=[C:24]([Cl:26])[CH:23]=[CH:22][C:3]=1[C:4]([NH:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[CH:18]([CH3:19])[CH2:17][C:16](=[O:20])[NH:15][N:14]=2)=[CH:9][C:8]=1[OH:21])=O.C1(C)C=CC(S(O)(=O)=O)=CC=1.C(O)(=O)C>O>[Cl:1][C:2]1[C:3]([C:4]2[O:21][C:8]3[CH:9]=[C:10]([C:13]4[CH:18]([CH3:19])[CH2:17][C:16](=[O:20])[NH:15][N:14]=4)[CH:11]=[CH:12][C:7]=3[N:6]=2)=[CH:22][CH:23]=[C:24]([Cl:26])[N:25]=1

참가 물질

5

반응물 3

HCID 176Acetic Acid2회HCID 6101p-Toluenesulfonic acidHCID 866890692,6-dichloro-N-[2-hydroxy-4-(4-methyl-6-oxo-1,4,5,6-tetrahydro-pyridazin-3-yl)-phenyl]-nicotinamide

생성물 1

HCID 179935426-[2-(2,6-dichloro-pyridin-3-yl)-benzoxazol-6-yl]-5-methyl-4,5-dihydro-2H-pyridazin-3-one

시약·촉매·용매 1

HCID 962Water용매

실험 절차

5.8 g (0.015 mol) 2,6-dichloro-N-[2-hydroxy-4-(4-methyl-6-oxo-1,4,5,6-tetrahydro-pyridazin-3-yl)-phenyl]-nicotinamide, 0.6 g para-toluenesulphonic acid and 60 ml glacial acetic acid are refluxed together for 15 h, then 40 ml glacial acetic acid are eliminated in vacuo and the residue is mixed with water. The precipitate formed is filtered off, washed with ethanol and then recrystallised from dioxane/DMF.

후처리

  1. customThe precipitate formed
  2. filtrationis filtered off
  3. washwashed with ethanol
  4. customrecrystallised from dioxane/DMF

출처 및 근거

ORD 기록
ord-4a5c6050643142db82953a27704bf795
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772323B2

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