Potassium Carbonate → 1-(2-(Piperidin-1-YL)ethyl)-1H-imidazol-2-amine

HRID 222633

반응식

HRID 222633 반응식
S(O)(O)(=O)=O.[NH2:6][C:7]1[NH:8][CH:9]=[CH:10][N:11]=1.C(=O)([O-])[O-].[K+].[K+].Cl.Cl[CH2:20][CH2:21][N:22]1[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1>CN(C=O)C>[N:22]1([CH2:21][CH2:20][N:8]2[CH:9]=[CH:10][N:11]=[C:7]2[NH2:6])[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 74826Piperidine, 1-(2-chloroethyl)-, hydrochlorideHCID 135136Bis(2-amino-1H-imidazole) sulphate

생성물 1

HCID 534024741-(2-(Piperidin-1-YL)ethyl)-1H-imidazol-2-amine수율 22.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

2-Aminoimidazole monosulfate (500 mg, 1.89 mmol) and potassium carbonate (580 mg, 4.16 mmol) were suspended in DMF (2 mL) and chloroethyl piperidine mono hydrochloride (766 mg, 4.16 mmol) was added. The reaction was heated at 100° C. for 2.5 hours before being cooled to room temperature and filtered. The filtrate was concentrated and purified by column chromatography (95:4.5:0.5 dichloromethane:methanol:aqueous ammonia) and the product was isolated as a brown oil (83 mg, 11%).

후처리

  1. temperaturebefore being cooled to room temperature
  2. filtrationfiltered
  3. concentrationThe filtrate was concentrated
  4. custompurified by column chromatography (95:4.5:0.5 dichloromethane:methanol:aqueous ammonia)

출처 및 근거

ORD 기록
ord-5a74d01fdcd14d459f877a5ccbc1b94d
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08207334B2

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