Sodium Hydroxide → 1,2,2,6,6-Pentamethyl-4-piperidone oxide

HRID 377367

반응식

HRID 377367 반응식
I.[CH3:2][N:3]1[C:8]([CH3:10])([CH3:9])[CH2:7][C:6](=[O:11])[CH2:5][C:4]1([CH3:13])[CH3:12].Cl.N[OH:16].[OH-].[Na+]>O>[CH3:2][N+:3]1([O-:16])[C:8]([CH3:9])([CH3:10])[CH2:7][C:6](=[O:11])[CH2:5][C:4]1([CH3:13])[CH3:12]

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 223975731,2,2,6,6-Pentamethyl-4-piperidone hydroiodide

생성물 1

HCID 193586881,2,2,6,6-Pentamethyl-4-piperidone oxide수율 84.1%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

A suspension of 1,2,2,6,6-pentamethyl-4-piperidone hydroiodide (3 g, 10.0 mmol) and hydroxylamine hydrochloride (980 mg, 14 mmol) in water (6 ml) was stirred at RT for 15 min. Solid NaOH was added until basic pH and thickening of the suspension. Water (3 ml) was added and stirring at RT was continued overnight. The suspension was filtered and the solid washed with water (few ml) and dried. The solid was then dissolved in Et2O, the solution was dried (MgSO4) and concentrated to give after drying pure title compound (1.55 g, 8.41 mmol, yield 83.3%) as white crystals.

후처리

  1. stirringstirring at RT
  2. waitwas continued overnight
  3. filtrationThe suspension was filtered
  4. washthe solid washed with water (few ml)
  5. customdried
  6. dissolutionThe solid was then dissolved in Et2O
  7. dry with materialthe solution was dried (MgSO4)
  8. concentrationconcentrated
  9. customto give

출처 및 근거

ORD 기록
ord-4092f7a061de4dd6b27612bb696f51e2
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06025390

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