Hydrochloric Acid → 1-Amino-4-methylpentan-2-one hydrochloride

HRID 1670529ノート

反応式

HRID 1670529 の反応式
[CH3:1][CH:2]([CH3:18])[CH2:3][C:4](=[O:17])[CH2:5][N:6]1C(=O)C2C(=CC=CC=2)C1=O.[ClH:19]>C(O)(=O)C.O>[ClH:19].[NH2:6][CH2:5][C:4](=[O:17])[CH2:3][CH:2]([CH3:18])[CH3:1]

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 70388412-(4-methyl-2-oxopentyl)-1H-isoindole-1,3(2H)-dione

生成物 1

HCID 137017551-Amino-4-methylpentan-2-one hydrochloride収率 81%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

実験手順

Slurry 2-(4-methyl-2-oxo-pentyl)-isoindole-1,3-dione (2.8 g, 11.4 mmol) in concentrated HCl (18 mL), glacial acetic acid (16 mL) and water (13 mL). Stir the mixture at reflux for 16 h. Cool to room temperature and pour the solution onto ice (25 mL). Filter off the solids, wash the filtrate with cold water (20 mL) and concentrate in vacuo to a solid. Recrystallize the solid in ethanol (15 mL) and diethyl ether (50 mL). Decant off the solvent and dry the white paste under reduced pressure to obtain the desired intermediate as a white solid (1.4 g, 81%).

後処理

  1. temperatureat reflux for 16 h
  2. additionpour the solution onto ice (25 mL)
  3. filtrationFilter off the solids
  4. washwash the filtrate with cold water (20 mL)
  5. concentrationconcentrate in vacuo to a solid
  6. customRecrystallize the solid in ethanol (15 mL)
  7. customDecant off the solvent
  8. customdry the white paste under reduced pressure

出典と根拠

ORDレコード
ord-f1bb7b21e6ea49529d86b787c1a95764
出典データセット
uspto-grants-2011_08
特許番号
US07994163B2

反応ノート

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