Hydrochloric Acid → HCID 20078040、化合物

HRID 1654478ノート

反応式

HRID 1654478 の反応式
Cl[C:2]1[N:6]([CH:7]([CH3:9])[CH3:8])[C:5]2[CH:10]=[CH:11][C:12]([Cl:14])=[CH:13][C:4]=2[N:3]=1.[CH3:15][N:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1.Cl>>[Cl:14][C:12]1[CH:11]=[CH:10][C:5]2[N:6]([CH:7]([CH3:9])[CH3:8])[C:2]([N:19]3[CH2:20][CH2:21][N:16]([CH3:15])[CH2:17][CH2:18]3)=[N:3][C:4]=2[CH:13]=1

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 531671-MethylpiperazineHCID 20078039HCID 20078039、化合物

生成物 1

HCID 20078040HCID 20078040、化合物収率 46.9%

反応条件

温度
140 °C

実験手順

A mixture of 2,5-dichloro-1-isopropylbenzimidazole (7 g) and N-methylpiperazine (10 g) was stirred at 140° C. for 3.5 hours. After cooling, 2N hydrochloric acid was added to the mixture and the mixture was washed with ethyl acetate. The 2N hydrochloric acid layer was made basic with an aqueous 2N sodiumhydroxide solution and extracted with ethyl acetate. The ethyl acetate layer was washed with a saturated sodium chloride solution 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)benzimidazole (4.2 g). A part of the obtained product was recrystallized from acetonitrile, which showed the following physical properties:

後処理

  1. temperatureAfter cooling
  2. washthe mixture was washed with ethyl acetate
  3. extractionextracted with ethyl acetate
  4. washThe ethyl acetate layer was washed with a saturated sodium chloride solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-bbbca3b7e749445bbd1b5ce1dea5c822
出典データセット
uspto-grants-1995_04
特許番号
US05407936

反応ノート

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