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

HRID 1619978ノート

反応式

HRID 1619978 の反応式
[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

参加物

5

反応物 3

HCID 176Acetic Acid2 回HCID 6101p-Toluenesulfonic acidHCID 866890692,6-dichloro-N-[2-hydroxy-4-(4-methyl-6-oxo-1,4,5,6-tetrahydro-pyridazin-3-yl)-phenyl]-nicotinamide

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-4a5c6050643142db82953a27704bf795
出典データセット
uspto-grants-2014_07
特許番号
US08772323B2

反応ノート

読み込み中…