Sodium Hydroxide → beta-Piperidinopropiophenone oxime

HRID 35012

반응식

HRID 35012 반응식
Cl.[N:2]1([CH2:8][CH2:9][C:10]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=O)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.Cl.[NH2:19][OH:20].C(=O)([O-])O.[Na+].[OH-].[Na+]>O.[Ag]>[N:2]1([CH2:8][CH2:9][C:10](=[N:19][OH:20])[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1

참가 물질

7

반응물 4

HCID 14798Sodium HydroxideHCID 701713-Piperidinopropiophenone hydrochlorideHCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium Bicarbonate

생성물 1

HCID 23906289beta-Piperidinopropiophenone oxime수율 74.8%

시약·촉매·용매 2

HCID 23954Silver촉매HCID 962Water용매2회

실험 절차

In 470 ml of water were dissolved 60.2 g of β-piperidinopropiophenone hydrochloride and 18.1 g of hydroxylamine hydrochloride. To this solution was added portionwise 21.9 g of sodium hydrogencarbonate. After the whole amount was added, the mixture was stirred overnight. To the stirred mixture was then added an aqueous solution of 14.2 g of sodium hydroxide in 47 ml of water. Thus obtained mixture was well stirred and allowed to stand for 2 hours to produce a white precipitate. The precipitate was collected by filtration and washed successively with two portions of 200 ml of water and ethanol. The washed precipitate was dried to obtain a white solid. The solid was then recrystallized from methanol to obtain 41.2 g (yield: 74.8%) of the subject compound as a silver-white scaly product.

후처리

  1. additionAfter the whole amount was added
  2. stirringThus obtained mixture was well stirred
  3. waitto stand for 2 hours
  4. customto produce a white precipitate
  5. filtrationThe precipitate was collected by filtration
  6. washwashed successively with two portions of 200 ml of water and ethanol
  7. customThe washed precipitate was dried
  8. customto obtain a white solid
  9. customThe solid was then recrystallized from methanol

출처 및 근거

ORD 기록
ord-e9c738adc29e404d9db764e041f0902d
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04764617

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