Hydrogen Bromide → HCID 19353953, 화합물

HRID 741730노트

반응식

HRID 741730 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 19353953HCID 19353953, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c28f541c939c45ff9039bc35ecd859cf
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05552426

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