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

HRID 222633

反応式

HRID 222633 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-5a74d01fdcd14d459f877a5ccbc1b94d
出典データセット
uspto-grants-2012_06
特許番号
US08207334B2

関連ノート

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