二甲基对苯二胺二盐酸 → beta-Piperidinopropiophenone oxime

HRID 35012

反应方程式

HRID 35012 反应方程式
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

参与物

7

反应物 4

HCID 14798二甲基对苯二胺二盐酸HCID 70171BETA-吡咯烷苯丙酮盐酸盐HCID 443297盐酸羟胺HCID 516892碳酸氢钠

产物 1

HCID 23906289beta-Piperidinopropiophenone oxime收率 74.8%

试剂、催化剂与溶剂 2

HCID 23954银(II)催化剂HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂2 次

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-e9c738adc29e404d9db764e041f0902d
来源数据集
uspto-grants-1988_08
专利号
US04764617

关联笔记

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