Sodium Hydroxide → beta-Piperidinopropiophenone oxime

HRID 35012

反応式

HRID 35012 の反応式
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

参加物

7

反応物 4

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

生成物 1

HCID 23906289beta-Piperidinopropiophenone oxime収率 74.8%

試薬・触媒・溶媒 2

HCID 23954Silver触媒HCID 962Water溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e9c738adc29e404d9db764e041f0902d
出典データセット
uspto-grants-1988_08
特許番号
US04764617

関連ノート

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