Hydrochloric Acid → Phenol, 4-nitro-2-(trifluoromethyl)-

HRID 28245

반응식

HRID 28245 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[C:11]([F:14])([F:13])[F:12].[OH-:15].[K+].Cl>CO.[Cl-].C([N+](CC)(CC)CC)C>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([OH:15])=[C:3]([C:11]([F:14])([F:13])[F:12])[CH:4]=1)([O-:10])=[O:9]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 612132-Chloro-5-nitrobenzotrifluoride

생성물 1

HCID 3014014Phenol, 4-nitro-2-(trifluoromethyl)-

시약·촉매·용매 2

HCID 5946Tetraethylammonium Chloride촉매HCID 887Methanol용매

반응 조건

온도
80 °C

실험 절차

450 g of 2-chloro-5-nitro-benzotrifluoride in 1,250 ml of methanol and 35 g of tetraethylammonium chloride are initially introduced. 1,000 g of an aqueous, 50% strength potassium hydroxide solution are then added dropwise (1 hour), the temperature being kept at a maximum of 40° C. by cooling. About 30 minutes after the addition has ended, the mixture is heated to 80° C. for 6 hours, cooled and rendered acid with concentrated hydrochloric acid. The mixture is extracted several times with 300 ml of methylene chloride each time, and the organic phase is dried with sodium sulphate and freed from the solvent under reduced pressure. About 413 g of crude product, melting point: 90°-95° C., are obtained with a purity of about 95% according to analysis by gas chromatography. After recrystallisation from toluene, or distillation under 0.5 mm, pure 4-nitro-2-trifluoromethylphenol is obtained, melting point: 134° C.

후처리

  1. custombeing kept at a maximum of 40° C.
  2. temperatureby cooling
  3. additionAbout 30 minutes after the addition
  4. temperaturecooled
  5. extractionThe mixture is extracted several times with 300 ml of methylene chloride each time
  6. dry with materialthe organic phase is dried with sodium sulphate
  7. customAbout 413 g of crude product, melting point: 90°-95° C., are obtained with a purity of about 95%
  8. customAfter recrystallisation
  9. distillationfrom toluene, or distillation under 0.5 mm

출처 및 근거

ORD 기록
ord-65f8aedb14bb489f9cd955c8f6bc1dcc
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04225731

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