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

HRID 746276ノート

反応式

HRID 746276 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 7909Methyl Isobutyl Ketone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b8d60fe6fb334e1a90e7ab6a5fe2b16d
出典データセット
uspto-grants-1986_07
特許番号
US04603201

反応ノート

読み込み中…