HCID 66988335、化合物 → 3-(5-methyl-1H-imidazol-4-yl)propanoic acid hydrochloride

HRID 530696ノート

反応式

HRID 530696 の反応式
[ClH:1].[CH3:2][C:3]1[NH:7][CH:6]=[N:5][C:4]=1/[CH:8]=[CH:9]/[C:10]([OH:12])=[O:11]>[Pd].O1CCCC1.O>[ClH:1].[CH3:2][C:3]1[NH:7][CH:6]=[N:5][C:4]=1[CH2:8][CH2:9][C:10]([OH:12])=[O:11]

参加物

4

反応物 1

HCID 66988335HCID 66988335、化合物

生成物 1

HCID 669882033-(5-methyl-1H-imidazol-4-yl)propanoic acid hydrochloride収率 83%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 21881883Oxolane--water (1/1)溶媒

実験手順

60 mg of 10% palladium-on-charcoal are introduced into a solution of 387 mg (2.1 mmol) of (E)-3-(5-methyl-1H-imidazol-4-yl)acrylic acid hydrochloride in 8 ml of 1/1 tetrahydrofuran/water, purged beforehand with nitrogen. The reaction medium is placed under a hydrogen atmosphere and then stirred for 19 hours. After filtering through Celite and rinsing thoroughly with dichloromethane, the recovered filtrate is concentrated under vacuum. The crude residue is taken up in toluene and concentrated again in order to remove the residual water, and is then taken up in a mixture of heptane and diisopropyl ether (80/20) with stirring for about 2 hours. The desired product precipitates and is filtered off under vacuum. 326 mg (83%) of 3-(5-methyl-1H-imidazol-4-yl)propanoic acid hydrochloride are obtained in the form of a white solid.

後処理

  1. custompurged
  2. filtrationAfter filtering through Celite
  3. washrinsing thoroughly with dichloromethane
  4. concentrationthe recovered filtrate is concentrated under vacuum
  5. concentrationconcentrated again in order
  6. customto remove the residual water
  7. additionis then taken up in a mixture of heptane and diisopropyl ether (80/20)
  8. stirringwith stirring for about 2 hours
  9. customThe desired product precipitates
  10. filtrationis filtered off under vacuum

出典と根拠

ORDレコード
ord-65df8d2f79404a06a63254122210c8c7
出典データセット
uspto-grants-2016_05
特許番号
US09353083B2

反応ノート

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