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

HRID 894927노트

반응식

HRID 894927 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b1e5a1dc92524fb4877fa7ae49592b0b
출처 데이터셋
uspto-grants-1981_08
특허 번호
US04285723

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