Hydrochloric Acid → 2-Chloro-1-(2,4-difluoro-5-methylphenyl)ethan-1-one

HRID 1784936

反応式

HRID 1784936 の反応式
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[CH3:9].[Al+3].[Cl-].[Cl-].[Cl-].[Cl:14][CH2:15][C:16](Cl)=[O:17].Cl>CCOC(C)=O.O>[Cl:14][CH2:15][C:16]([C:5]1[CH:4]=[C:3]([CH3:9])[C:2]([F:1])=[CH:7][C:6]=1[F:8])=[O:17]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 6577Chloroacetyl chlorideHCID 679832,4-Difluoro-1-methylbenzeneHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 739948662-Chloro-1-(2,4-difluoro-5-methylphenyl)ethan-1-one

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

To a stirring solution of 2,4-difluorotoluene was added 6.3 g (47.3 mmol) of AlCl3, and 3.4 mL (42.6 mmol) of chloroacetyl chloride at 0° C. After the mixture was stirred for 10 min. at 0° C. and then at 45° C. for 30 min. The mixture was allowed to cool to r.t., about 16 mL of conc. HCl, 25 mL of water, and 100 mL of EtOAc were added. The organic layer was separated and washed with brine and sat. NaHCO3 (2×), and dried over Na2SO4. The solution was filtered and concentrated to give 9.0 g of 2-chloro-1-(2,4-difluoro-5-methylphenyl)ethanone as a colorless solid that was used without further purification.

後処理

  1. waitat 45° C. for 30 min
  2. temperatureto cool to r.t.
  3. customThe organic layer was separated
  4. washwashed with brine and sat. NaHCO3 (2×)
  5. dry with materialdried over Na2SO4
  6. filtrationThe solution was filtered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-8235be2de36244b5931c0eec595e522e
出典データセット
uspto-grants-2009_03
特許番号
US07504420B2

関連ノート

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