Ethyl Acetate → HCID 15291316, 화합물

HRID 1654483노트

반응식

HRID 1654483 반응식
Cl[C:2]1[N:6]([CH:7]([CH3:9])[CH3:8])[C:5]2[CH:10]=[C:11]([N+:15]([O-:17])=[O:16])[C:12]([Cl:14])=[CH:13][C:4]=2[N:3]=1.[CH3:18][N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1.C(OCC)(=O)C>C1(C)C=CC=CC=1>[Cl:14][C:12]1[C:11]([N+:15]([O-:17])=[O:16])=[CH:10][C:5]2[N:6]([CH:7]([CH3:9])[CH3:8])[C:2]([N:22]3[CH2:23][CH2:24][N:19]([CH3:18])[CH2:20][CH2:21]3)=[N:3][C:4]=2[CH:13]=1

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 531671-MethylpiperazineHCID 20078042HCID 20078042, 화합물

생성물 1

HCID 15291316HCID 15291316, 화합물수율 84.7%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

2,5-Dichloro-1-isopropyl-6-nitrobenzimidazole (4.6 g) was suspended in toluene (31 ml) and to the suspension was added dropwise N-methylpiperazine (8.4 g) and then the mixture was refluxed for 30 minutes. To the reaction solution was added ethyl acetate and the mixture was washed with water and then extracted with 2N hydrochloric acid. The water layer was separated and made basic with an aqueous sodium hydroxide solution and then extracted with ethyl acetate. The organic layer was washed with water and dried over anhydrous magnesium sulfate and then the solvent was distilled off under reduced pressure to give 5-chloro-1-isopropyl-2-(4-methyl-1-piperazinyl)-6-nitrobenzimidazole (4.8 g). A part of the obtained product was recrystallized from acetonitrile, which showed the physical properties consistent with those in Preparation 8.

후처리

  1. temperaturethe mixture was refluxed for 30 minutes
  2. washthe mixture was washed with water
  3. extractionextracted with 2N hydrochloric acid
  4. customThe water layer was separated
  5. extractionextracted with ethyl acetate
  6. washThe organic layer was washed with water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-bae5fce7ebe4445f882e8bb7df32a212
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05407936

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