海萝胶 → N-(3,5-dimethylphenyl)-2-(hydroxyimino)acetamide

HRID 3107

反应方程式

HRID 3107 反应方程式
Cl[C:2](Cl)(Cl)[CH:3]([OH:5])O.S([O-])([O-])(=O)=O.[Na+].[Na+].[CH3:15][C:16]1[CH:17]=[C:18]([CH:20]=[C:21]([CH3:23])[CH:22]=1)[NH2:19].Cl.Cl.[NH2:26][OH:27]>O>[CH3:15][C:16]1[CH:17]=[C:18]([NH:19][C:3](=[O:5])[CH:2]=[N:26][OH:27])[CH:20]=[C:21]([CH3:23])[CH:22]=1

参与物

7

反应物 5

HCID 313海萝胶HCID 2707水合氯醛HCID 79491-氨基-3,5-二甲苯HCID 24436无水硫酸钠HCID 443297盐酸羟胺

产物 1

HCID 53405864N-(3,5-dimethylphenyl)-2-(hydroxyimino)acetamide收率 95%

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂3 次

实验过程

To a solution of chloral hydrate (14.1 g, 85.24 mM) and sodium sulfate (88.2g, 7.53 eq.) in 270 mL of water was added a solution of 3,5-dimethylaniline in a solution of concentrated HCl (16 mL) and water (51 mL), whereupon an off-white precipitate formed. The mixture was stirred for 10 min prior to adding an aqueous solution of hydroxylamine hydrochloride (17.4 g, 250 mM) in water (50 mL) and then heated at reflux for 10 min during which time the solids dissolved and a tan precipitate formed. The mixture was cooled and filtered, and the collected solids were air dried to yield the title compound (15.0 g, 95%).

后处理

  1. customwhereupon an off-white precipitate formed
  2. temperatureheated
  3. temperatureat reflux for 10 min during which time the solids
  4. dissolutiondissolved
  5. customa tan precipitate formed
  6. temperatureThe mixture was cooled
  7. filtrationfiltered
  8. customdried

来源与证据

ORD记录
ord-5139598c1f4b45d2b198d2ebd6c62ba7
来源数据集
uspto-grants-1998_03
专利号
US05733910

关联笔记

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