Water → 2-Chloro-5-(2-chloro-4-trifluoromethylphenoxy)benzoic acid

HRID 894927ノート

反応式

HRID 894927 の反応式
[Cl:1][C:2]1[CH:17]=[C:16]([C:18]([F:21])([F:20])[F:19])[CH:15]=[CH:14][C:3]=1[O:4][C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][CH:13]=1)[C:8]([OH:10])=[O:9].[Cl:22]Cl.O>C(O)(=O)C>[Cl:22][C:11]1[CH:12]=[CH:13][C:5]([O:4][C:3]2[CH:14]=[CH:15][C:16]([C:18]([F:20])([F:19])[F:21])=[CH:17][C:2]=2[Cl:1])=[CH:6][C:7]=1[C:8]([OH:10])=[O:9]

参加物

5

反応物 3

HCID 962WaterHCID 24526ChlorineHCID 916853-[2-Chloro-4-(trifluoromethyl)phenoxy]benzoic acid

生成物 1

HCID 130136822-Chloro-5-(2-chloro-4-trifluoromethylphenoxy)benzoic acid

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 3(2-chloro-4-trifluoromethylphenoxy)benzoic acid (5 g) in glacial acetic acid (30 ml) was heated under reflux while chlorine was passed through the solution for 5 hours. The solution was left to stand for two days at room temperature and then poured into cold water (500 ml). An off-white gummy solid separated. This was extracted with ethyl acetate and the extract dried and evaporated. The brown oil remaining was dissolved in sodium bicarbonate solution and the solution extracted with ethyl acetate. The aqueous solution was acidified with hydrochloric acid. The solution was decanted from the precipitated gum, and the gum taken up in boiling hexane. The hexane solution was filtered and allowed to cool. The required 2-chloro-5(2-chloro-4-trifluoromethylphenoxy)benzoic acid was obtained (1.0 g) as crystals of melting point 103°-104°. This acid was used as starting material for compounds 7 and 8.

後処理

  1. waitThe solution was left
  2. waitto stand for two days at room temperature
  3. customAn off-white gummy solid separated
  4. extractionThis was extracted with ethyl acetate
  5. customthe extract dried
  6. customevaporated
  7. dissolutionThe brown oil remaining was dissolved in sodium bicarbonate solution
  8. extractionthe solution extracted with ethyl acetate
  9. customThe solution was decanted from the precipitated gum
  10. filtrationThe hexane solution was filtered
  11. temperatureto cool

出典と根拠

ORDレコード
ord-b1e5a1dc92524fb4877fa7ae49592b0b
出典データセット
uspto-grants-1981_08
特許番号
US04285723

反応ノート

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