Aldoxime → Acetonitrile oxide

HRID 1606003ノート

反応式

HRID 1606003 の反応式
ClCl.[CH:3](=[N:5][OH:6])[CH3:4].C(=O)(O)[O-].[Na+].[Cl:12][C:13]1[C:14](=[O:21])[CH:15]=[CH:16][C:17](=[O:20])[C:18]=1[Cl:19]>O>[C:3](#[N+:5][O-:6])[CH3:4].[Cl:12][C:13]1[C:14](=[O:21])[C:15]2[C:3]([CH3:4])=[N:5][O:6][C:16]=2[C:17](=[O:20])[C:18]=1[Cl:19]

参加物

7

反応物 4

HCID 7863AldoximeHCID 24526ChlorineHCID 1384232,3-Dichloro-1,4-benzoquinoneHCID 516892Sodium Bicarbonate

生成物 2

HCID 522391Acetonitrile oxideHCID 21545721HCID 21545721、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of acetonitrile oxide was prepared by passing chlorine (10.8 grams) over 30 minutes into a stirred suspension of acetaldoxime (9 grams) and sodium bicarbonate (25.2 grams) in water at 0° C was added 2,3-dichlorobenzoquinone (17.7 grams) portionwise over 15 minutes. The mixture was stirred at 0°-5° C for 2 hours and then extracted with methylene chloride. The dried extracts were evaporated to dryness under reduced pressure and the residue recrystallized from ethanol to give the desired product as yellow crystals having a melting point of 214°-215° C.

後処理

  1. customover 30 minutes
  2. extractionextracted with methylene chloride
  3. customThe dried extracts were evaporated to dryness under reduced pressure
  4. customthe residue recrystallized from ethanol

出典と根拠

ORDレコード
ord-a707d3f725624214a4ace320b4d506a7
出典データセット
uspto-grants-1976_04
特許番号
US03952003

反応ノート

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