Potassium Chloride → HCID 178472876, 화합물

HRID 745882

반응식

HRID 745882 반응식
[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]

참가 물질

6

반응물 3

HCID 4873Potassium ChlorideHCID 8868Ethyl AcetoacetateHCID 23668193Sodium Nitrite

생성물 1

HCID 178472876HCID 178472876, 화합물수율 86.5%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-50cc48fa41b34310a64b563af2d4f7bb
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04600772

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