Sulfuric Acid → Diethyl (3-chloro-2,4-difluorobenzoyl)malonate

HRID 1449839

반응식

HRID 1449839 반응식
[Mg].[C:2]([O:10][CH2:11][CH3:12])(=[O:9])[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].[Cl:13][C:14]1[C:15]([F:24])=[C:16]([CH:20]=[CH:21][C:22]=1[F:23])[C:17](Cl)=[O:18].S(=O)(=O)(O)O>C(O)C.C1(C)C=CC=CC=1.C(Cl)(Cl)(Cl)Cl>[Cl:13][C:14]1[C:15]([F:24])=[C:16]([CH:20]=[CH:21][C:22]=1[F:23])[C:17]([CH:3]([C:4]([O:6][CH2:7][CH3:8])=[O:5])[C:2]([O:10][CH2:11][CH3:12])=[O:9])=[O:18]

참가 물질

8

반응물 4

HCID 1118Sulfuric AcidHCID 7761Diethyl MalonateHCID 27735383-Chloro-2,4-difluorobenzoyl chlorideHCID 5462224Magnesium

생성물 1

HCID 22077280Diethyl (3-chloro-2,4-difluorobenzoyl)malonate

시약·촉매·용매 3

HCID 702Ethanol용매2회HCID 1140Toluene용매HCID 5943Carbon Tetrachloride용매

반응 조건

온도
60 °C

실험 절차

3.9 g (0.16 mol) of magnesium are initially introduced into 8.6 ml of ethanol and the reaction is started with carbon tetrachloride. A solution of 23.1 g (0.144 mol) of diethyl malonate in 16.3 ml of ethanol is added dropwise at an internal temperature of 50°-60° C. such that this temperature is maintained. The mixture is then subsequently stirred at 60° C. for one hour. Thereafter, a solution of 31.3 g (0.148 mol) of 3-chloro-2,4-difluorobenzoyl chloride in 16 ml of toluene is added dropwise at -10° to -5° C. and the mixture is subsequently stirred at 0° C. for one hour and then overnight, while warming to room temperature. The reaction mixture is poured onto ice-water, acidified with 10 ml of concentrated sulphuric acid and extracted with toluene. The extract is washed with saturated sodium chloride solution and the solvent is removed in vacuo.

후처리

  1. temperatureis maintained
  2. stirringthe mixture is subsequently stirred at 0° C. for one hour
  3. temperatureovernight, while warming to room temperature
  4. additionThe reaction mixture is poured onto ice-water
  5. extractionextracted with toluene
  6. washThe extract is washed with saturated sodium chloride solution
  7. customthe solvent is removed in vacuo

출처 및 근거

ORD 기록
ord-af8b5f66174c455397287bf8f4c8131d
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05599980

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