Hydrochloric Acid → 1-methyl-2-(piperazin-1-yl)-1H-benzo[d]imidazole

HRID 2415863ノート

反応式

HRID 2415863 の反応式
Cl[C:2]1[N:6]([CH3:7])[C:5]2[CH:8]=[CH:9][CH:10]=[CH:11][C:4]=2[N:3]=1.[NH:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1.Cl>O>[CH3:7][N:6]1[C:5]2[CH:8]=[CH:9][CH:10]=[CH:11][C:4]=2[N:3]=[C:2]1[N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 4837PiperazineHCID 6630802-chloro-1-methyl-1H-1,3-benzodiazole

生成物 1

HCID 6675511-methyl-2-(piperazin-1-yl)-1H-benzo[d]imidazole

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
150 °C

実験手順

A mixture of 1 g (6.02 mmol) of 2-chloro-1-methyl-benzimidazole and 2.58 g (30 mmol) of piperazine is heated to 150° C. without a solvent. The cooled melt is combined successively with water and dilute hydrochloric acid and extracted with dichloromethane. Then the aqueous phase is made alkaline with dilute sodium hydroxide solution and extracted with dichloromethane. The organic phase is dried over sodium sulphate and concentrated by evaporation. The product is purified by column chromatography on silica gel (eluant: dichloromethane/ethanol/ammonia=5:1:0.1).

後処理

  1. extractionextracted with dichloromethane
  2. extractionextracted with dichloromethane
  3. dry with materialThe organic phase is dried over sodium sulphate
  4. concentrationconcentrated by evaporation
  5. customThe product is purified by column chromatography on silica gel (eluant: dichloromethane/ethanol/ammonia=5:1:0.1)

出典と根拠

ORDレコード
ord-2fa0de9281d94d13a7aafd0340a3f084
出典データセット
uspto-grants-2004_11
特許番号
US06821967B2

反応ノート

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