Ammonia → 2,5'-Bi-1H-benzimidazole, 1-methyl-2'-propyl-

HRID 1081891ノート

反応式

HRID 1081891 の反応式
S(O)(O)(=O)=O.[CH2:6]([C:9]1[NH:10][C:11]2[CH:17]=[C:16]([C:18](O)=O)[CH:15]=[CH:14][C:12]=2[N:13]=1)[CH2:7][CH3:8].C([C:24]1[NH:25][C:26]2[CH:32]=[C:31](C(O)=O)[CH:30]=[CH:29][C:27]=2[N:28]=1)CC.Cl.Cl.CNC1C=CC=CC=1N.N>O>[CH2:6]([C:9]1[NH:10][C:11]2[CH:17]=[C:16]([C:18]3[N:25]([CH3:24])[C:26]4[CH:32]=[CH:31][CH:30]=[CH:29][C:27]=4[N:28]=3)[CH:15]=[CH:14][C:12]=2[N:13]=1)[CH2:7][CH3:8]

参加物

5

反応物 3

HCID 222AmmoniaHCID 91296N-Methyl-o-phenylenediamine dihydrochlorideHCID 856442212-n-Propyl-benzimidazole-5-carboxylic acid-hemisulphate

生成物 1

HCID 104694762,5'-Bi-1H-benzimidazole, 1-methyl-2'-propyl-

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 6.7 g (25 mMol) of 2-n-propyl-benzimidazole-5-carboxylic acid-hemisulphate and 4.9 g (25 mMol) of 2-methylaminoaniline-dihydrochloride in 200 g of polyphosphoric acid is stirred for 5 hours at 150° C., then poured onto 600 ml of water and made alkaline with concentrated ammonia whilst cooling with ice. The resulting solution is extracted three times with 200 ml of ethyl acetate, the crude product thus obtained is purified by column chromatography (300 g of silica gel; eluant:methylene chloride/methanol=15:1).

後処理

  1. temperaturewhilst cooling with ice
  2. extractionThe resulting solution is extracted three times with 200 ml of ethyl acetate

出典と根拠

ORDレコード
ord-17489800f8014dd3a9fa3e6eb598427c
出典データセット
uspto-grants-1996_12
特許番号
US05587393

反応ノート

読み込み中…