Hydrogen Bromide → HCID 19353953、化合物

HRID 741730ノート

反応式

HRID 741730 の反応式
[C:1]1([N:7]2[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[N:9]=[C:8]2[C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([O:22]C)[CH:17]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Br>C(O)(=O)C>[C:1]1([N:7]2[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[N:9]=[C:8]2[C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([OH:22])[CH:17]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 260Hydrogen BromideHCID 193539742-(3-Methoxyphenyl)-1-phenyl-1H-benzimidazole

生成物 1

HCID 19353953HCID 19353953、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 1-phenyl-2-(3-methoxyphenyl)benzimidazole (0.20 g, 0.67 mmol) and hydrobromic acid (4 ml) and acetic acid (4 ml) was refluxed for 48 hours. The reaction mixture was cooled and extracted with diethyl ether (5×150 ml) at pH 3-5. The organic fractions were discarded. The aqueous phase was alkalinized to pH 8-9 and extracted with ethyl acetate (5×150 ml). The organic layers were combined, washed with a saturated sodium chloride solution, dried over magnesium sulfate, filtered, and the solvents were removed in vacuo to yield a white solid. The solid was triturated with an ethyl acetate/diethyl ether mixture.

後処理

  1. temperatureThe reaction mixture was cooled
  2. extractionextracted with diethyl ether (5×150 ml) at pH 3-5
  3. extractionextracted with ethyl acetate (5×150 ml)
  4. washwashed with a saturated sodium chloride solution
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customthe solvents were removed in vacuo
  8. customto yield a white solid
  9. customThe solid was triturated with an ethyl acetate/diethyl ether mixture

出典と根拠

ORDレコード
ord-c28f541c939c45ff9039bc35ecd859cf
出典データセット
uspto-grants-1996_09
特許番号
US05552426

反応ノート

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