Hydrochloride methanol → 5-[3-(Amino)propylamino]imidazo[1,2-a]pyridine dihydrochloride

HRID 5434

反応式

HRID 5434 の反応式
C(OC([NH:8][CH2:9][CH2:10][CH2:11][NH:12][C:13]1[N:18]2[CH:19]=[CH:20][N:21]=[C:17]2[CH:16]=[CH:15][CH:14]=1)=O)(C)(C)C.[ClH:22].CO>C(Cl)Cl>[ClH:22].[ClH:22].[NH2:8][CH2:9][CH2:10][CH2:11][NH:12][C:13]1[N:18]2[CH:19]=[CH:20][N:21]=[C:17]2[CH:16]=[CH:15][CH:14]=1

参加物

4

反応物 2

HCID 21893726Hydrochloride methanolHCID 23362879Carbamic acid,[3-(imidazo[1,2-a]pyridin-5-ylamino)propyl]-,1,1-dimethylethyl ester

生成物 1

HCID 200866655-[3-(Amino)propylamino]imidazo[1,2-a]pyridine dihydrochloride収率 83%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a suspension of 5-[3-(tert-butoxycarbonylamino)propylamino]imidazo[1,2-a]pyridine (1.742 g, 6 mmoles) in methylene chloride (40 ml) was added hydrogen chloride-methanol (6 ml) and the mixture was stirred at room temperature for 20 hours. After the solvent was distilled off, ethanol (15 ml) and ether (30 ml) were added to the residue. Then, the crystals precipitated were filtered off and washed in turn with ether and a small amount of ethanol to obtain 1.311 g of the desired product (83.0%, pale yellow crystals).

後処理

  1. distillationAfter the solvent was distilled off
  2. additionethanol (15 ml) and ether (30 ml) were added to the residue
  3. customThen, the crystals precipitated
  4. filtrationwere filtered off
  5. washwashed in turn with ether

出典と根拠

ORDレコード
ord-689b4b2ef67943d4b073104bea7fe4b7
出典データセット
uspto-grants-1993_09
特許番号
US05244908

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