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

HRID 1670529노트

반응식

HRID 1670529 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

HCID 137017551-Amino-4-methylpentan-2-one hydrochloride수율 81%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-f1bb7b21e6ea49529d86b787c1a95764
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07994163B2

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