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

HRID 2415863노트

반응식

HRID 2415863 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
150 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-2fa0de9281d94d13a7aafd0340a3f084
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06821967B2

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