Oxalic Acid → (E)-1-(2-Pyridyl)-2-[2-(4-pyridyl)ethenyl]-1H-benzimidazole oxalate

HRID 382588

反応式

HRID 382588 の反応式
[CH3:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=2)[C:5]2[CH:13]=[CH:14][CH:15]=[CH:16][C:4]=2[N:3]=1.[N:17]1[CH:22]=[CH:21][C:20]([CH:23]=O)=[CH:19][CH:18]=1.Cl.Cl.N1C=CC=CC=1N1C2C=CC=CC=2N=C1/C=C/C1C=CC=CN=1.[C:50]([OH:55])(=[O:54])[C:51]([OH:53])=[O:52]>CO>[C:50]([OH:55])(=[O:54])[C:51]([OH:53])=[O:52].[N:8]1[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=1[N:6]1[C:5]2[CH:13]=[CH:14][CH:15]=[CH:16][C:4]=2[N:3]=[C:2]1/[CH:1]=[CH:23]/[C:20]1[CH:21]=[CH:22][N:17]=[CH:18][CH:19]=1

参加物

6

反応物 4

HCID 971Oxalic AcidHCID 133894-PyridinecarboxaldehydeHCID 227366432-Methyl-1-(pyridin-2-yl)-1H-benzimidazoleHCID 22736657(E)-1-(2-Pyridyl)-2-[2-(2-pyridyl)ethenyl]-1H-benzimidazole dihydrochloride

生成物 1

HCID 22736688(E)-1-(2-Pyridyl)-2-[2-(4-pyridyl)ethenyl]-1H-benzimidazole oxalate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Free base of the titled compound was prepared from 2-methyl-1-(2-pyridyl)-1H-benzimidazole and pyridine-4-carboxaldehyde according to the preparation of (E)-1-(2-pyridyl)-2-[2-(2-pyridyl)ethenyl]-1H-benzimidazole dihydrochloride (Example 44). The free base and oxalic acid were dissolved into MeOH. Concentration and recrystallization from ethyl MeOH/Et2O/n-hexane yielded the titled compound.

後処理

  1. concentrationConcentration and recrystallization from ethyl MeOH/Et2O/n-hexane

出典と根拠

ORDレコード
ord-a99a7f94c89e4ff5a2e93daf4d425045
出典データセット
uspto-grants-2001_10
特許番号
US06310079B1

関連ノート

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