Hydrochloric Acid → 2-Nitro-4-(trifluoromethyl)phenol

HRID 28246

반응식

HRID 28246 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].[Cl-].C(CCCCCCCCCCCC[NH+](C)C)C1C=CC=CC=1.[OH-:38].[K+].Cl>COCCO>[N+:12]([C:3]1[CH:4]=[C:5]([C:8]([F:11])([F:10])[F:9])[CH:6]=[CH:7][C:2]=1[OH:38])([O-:14])=[O:13]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 84624-Chloro-alpha,alpha,alpha-trifluoro-3-nitrotolueneHCID 14797Potassium HydroxideHCID 53445721Benzyldodecyldimethyl ammonium chloride

생성물 1

HCID 98162-Nitro-4-(trifluoromethyl)phenol수율 92%

시약·촉매·용매 1

HCID 80192-Methoxyethanol용매

반응 조건

온도
65 °C

실험 절차

45 g of 4-chloro-3-nitro-benzotrifluoride and 10 ml of 50% strength aqueous benzyldodecyldimethylammonium chloride are initially introduced into 150 ml of ethylene glycol monomethyl ether, and 100 g of 50% strength potassium hydroxide solution are added dropwise in the course of about 30 minutes, up to a temperature of 65° C. The mixture is then stirred at 65° C. for 6 hours and subsequently cooled and rendered acid with concentrated hydrochloric acid, and about 500 ml of distillate are driven over with steam. The organic phase is separated off and washed with 20 ml of dilute hydrochloric acid, and the organic phase is again separated off and dried with sodium sulphate. 38 g of 2-nitro-4-trifluoromethylphenol are obtained, which corresponds to a yield of 92% of theory.

후처리

  1. additionare added dropwise in the course of about 30 minutes, up to a temperature of 65° C
  2. temperaturesubsequently cooled
  3. customThe organic phase is separated off
  4. washwashed with 20 ml of dilute hydrochloric acid
  5. customthe organic phase is again separated off
  6. dry with materialdried with sodium sulphate

출처 및 근거

ORD 기록
ord-dd14553770ba48f4a69e66321c63b24e
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04225731

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