Potassium Chloride → HCID 178472876、化合物

HRID 127983

反応式

HRID 127983 の反応式
[C:1]([O:7][CH2:8][CH3:9])(=[O:6])[CH2:2][C:3]([CH3:5])=[O:4].[N:10]([O-])=[O:11].[Na+].[Cl-].[K+]>C(O)(=O)C.O>[OH:11]/[N:10]=[C:2](/[C:3](=[O:4])[CH3:5])\[C:1]([O:7][CH2:8][CH3:9])=[O:6]

参加物

6

反応物 3

HCID 4873Potassium ChlorideHCID 8868Ethyl AcetoacetateHCID 23668193Sodium Nitrite

生成物 1

HCID 178472876HCID 178472876、化合物収率 86.5%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒2 回

実験手順

To a stirred and ice-cooled solution of ethyl acetoacetate (292 g) in glacial acetic acid (296 ml) was added a solution of sodium nitrite (180 g) in water (400 ml) at such a rate that the reaction temperature was maintained below 10° C. Stirring and cooling were continued for about 30 min., when a solution of potassium chloride (160 g) in water (800 ml) was added. The resulting mixture was stirred for one hour. The lower oily phase was separated and the aqueous phase was extracted with diethyl ether. The extract was combined with the oil, washed successively with water and saturated brine, dried, and evaporated. The residual oil, which solidified on standing, was washed with petrol and dried in vacuo over potassium hydroxide, giving ethyl (Z)-2-(hydroxyimino)-3-oxobutyrate (309 g).

後処理

  1. temperaturewas maintained below 10° C
  2. stirringStirring
  3. temperaturecooling
  4. stirringThe resulting mixture was stirred for one hour
  5. customThe lower oily phase was separated
  6. extractionthe aqueous phase was extracted with diethyl ether
  7. washwashed successively with water and saturated brine
  8. customdried
  9. customevaporated
  10. washwas washed with petrol
  11. dry with materialdried in vacuo over potassium hydroxide

出典と根拠

ORDレコード
ord-36b3af750628480eb347c96ded4d2e9c
出典データセット
uspto-grants-1981_03
特許番号
US04258041

関連ノート

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