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Hydrochloric Acid → 1H-Imidazole, 2-(2-benzofuranyl)-, monohydrochloride

HRID 1033550
ノート
印刷プレビュー

反応式

HRID 1033550 の反応式
CO[CH:3](OC)[CH2:4][NH2:5].[ClH:8].[O:9]1[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=2[CH:11]=[C:10]1[C:18](=[NH:21])OC.Cl>CO.C(OCC)C.C(O)C>[ClH:8].[O:9]1[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=2[CH:11]=[C:10]1[C:18]1[NH:21][CH:3]=[CH:4][N:5]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 89728Aminoacetaldehyde dimethyl acetalHCID 18962029HCID 18962029、化合物

生成物 1

HCID 30735951H-Imidazole, 2-(2-benzofuranyl)-, monohydrochloride

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 21585056Diethyl ether ethanol溶媒

反応条件

温度
60 °C

実験手順

A solution of aminoacetaldehyde dimethylacetal (7.3 g) and methyl benzofuran-2-carboximidate hydrochloride (13.4 g) in methanol (135 ml) was stirred at 60° C. for 16 hours. The mixture was then evaporated to dryness. Hydrochloric acid (750 ml, 2M) was added and the resulting mixture was stirred at 60° C. for 16 hours. After cooling, the solution was washed with dichloromethane. The aqueous layer was basified with sodium hydroxide and the free base was extracted with ethyl acetate. The organic layer was washed with saturated brine and dried. Evaporation of the solvent gave a solid residue which was dissolved in diethyl ether/ethanol. Ethereal HCl was added to solution and the precipitated salt was collected by filtration (12.5 g, 90%).

後処理

  1. customThe mixture was then evaporated to dryness
  2. additionHydrochloric acid (750 ml, 2M) was added
  3. temperatureAfter cooling
  4. washthe solution was washed with dichloromethane
  5. extractionthe free base was extracted with ethyl acetate
  6. washThe organic layer was washed with saturated brine
  7. customdried
  8. customEvaporation of the solvent
  9. customgave a solid residue which
  10. filtrationthe precipitated salt was collected by filtration (12.5 g, 90%)

出典と根拠

ORDレコード
ord-264b93231e6d4e349f1f6887c50fc973
出典データセット
uspto-grants-1994_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05310930

反応ノート

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