Hydrochloric Acid → 2-Chloro-4-(3,5-dichloro-4-methylphenyl)-4-oxobutyric acid

HRID 746276노트

반응식

HRID 746276 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:10](=[O:16])[CH:11]=[CH:12][C:13]([OH:15])=[O:14])[CH:5]=[C:6]([Cl:9])[C:7]=1[CH3:8].[ClH:17]>C(C(C)=O)C(C)C.O>[Cl:17][CH:12]([CH2:11][C:10]([C:4]1[CH:3]=[C:2]([Cl:1])[C:7]([CH3:8])=[C:6]([Cl:9])[CH:5]=1)=[O:16])[C:13]([OH:15])=[O:14]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 545341534-(3,5-Dichloro-4-methylphenyl)-4-oxobut-2-enoic acid

생성물 1

HCID 134203442-Chloro-4-(3,5-dichloro-4-methylphenyl)-4-oxobutyric acid수율 100%

시약·촉매·용매 2

HCID 962Water용매HCID 7909Methyl Isobutyl Ketone용매

실험 절차

A suspension of 5.18 g (0.02 mole) of 4-(3,5-dichloro-4-methylphenyl)-4-oxo-2-butenoic acid, prepared as described in Example 1(b), in 50 ml of methyl isobutyl ketone was saturated with dry hydrogen chloride gas, by blowing the gas through the suspension whilst ice-cooling and stirring it. The mixture was then stirred at room temperature for a further 1 hour, after which it was diluted with 30 ml of cold water and extracted with ethyl acetate. The extract was washed with water and then dried over anhydrous sodium sulphate, after which the solvent was distilled off and the residue was washed with a small amount of hexane and then dried, giving 5.91 g (yield 100%) of the desired 2-chloro-4-(3,5-dichloro-4-methylphenyl)-4-oxobutyric acid, melting at 129°-132° C.

후처리

  1. customprepared
  2. temperaturecooling
  3. stirringThe mixture was then stirred at room temperature for a further 1 hour
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with water
  6. dry with materialdried over anhydrous sodium sulphate
  7. distillationafter which the solvent was distilled off
  8. washthe residue was washed with a small amount of hexane
  9. customdried

출처 및 근거

ORD 기록
ord-b8d60fe6fb334e1a90e7ab6a5fe2b16d
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04603201

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