Sodium Hydroxide → 1,2,2,6,6-Pentamethyl-piperidin-4-one oxime

HRID 1070699

반응식

HRID 1070699 반응식
I.[CH3:2][N:3]1[C:8]([CH3:10])([CH3:9])[CH2:7][C:6](=O)[CH2:5][C:4]1([CH3:13])[CH3:12].Cl.[NH2:15][OH:16].[OH-].[Na+]>O>[CH3:2][N:3]1[C:8]([CH3:10])([CH3:9])[CH2:7][C:6](=[N:15][OH:16])[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 2419501,2,2,6,6-Pentamethyl-piperidin-4-one oxime수율 83.3%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

A suspension of 1,2,2,6,6-pentamethyl-4-piperidone hydroiodide (3 g, 10.1 mmol) and hydroxylamine hydrochloride (980 mg, 14 mmol) in water (6 ml) was stirred at RT for 15 minutes. 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-20f3f91506e544d7a8f2cfe8052b4ca4
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06903117B2

연결된 노트

불러오는 중…