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Hydrochloric Acid → 1-(3-(trifluoromethyl)phenyl)-1H-pyrazole

HRID 2198760
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HRID 2198760 반응식
[F:1][C:2]([F:12])([F:11])[C:3]1[CH:4]=[C:5]([NH:9][NH2:10])[CH:6]=[CH:7][CH:8]=1.O.Cl.C(O[CH:18](OCC)[CH2:19][CH:20](OCC)OCC)C>C(O)C>[F:1][C:2]([F:11])([F:12])[C:3]1[CH:4]=[C:5]([N:9]2[CH:20]=[CH:19][CH:18]=[N:10]2)[CH:6]=[CH:7][CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 671471,1,3,3-TetraethoxypropaneHCID 98650(3-(Trifluoromethyl)phenyl)hydrazine

생성물 1

HCID 130663261-(3-(trifluoromethyl)phenyl)-1H-pyrazole수율 80%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Into a 500 ml., 2-neck flask, fitted with a condenser and a magnetic stirrer, is successively added 35.2 g. (0.2 M.) of m-trifluoromethylphenyl hydrazine, 15 ml. of water, 20 ml. of 100% ethanol, 16.5 ml. of concentrated hydrochloric acid (slowly) and 44.0 g. (0.2 M.) of 1,1,3,3-tetraethoxypropane. The reaction mixture is then heated slowly to between 80° C. and 90° C., and after maintaining the mixture at this temperature range for a period of between 2 and 3 hours, the reaction mixture is cooled, quenched on ice water, extracted with ethylacetate and washed several times with water. After drying the organic solution over sodium sulfate, the solvent is evaporated on a rotary evaporator to obtain a very dark liquid which is then distilled at 70° to 80° C. and a pressure of about 100 microns to yield a light yellow oil (Yield: 80%).

후처리

  1. custom, 2-neck flask, fitted with a condenser and a magnetic stirrer
  2. temperatureThe reaction mixture is then heated slowly to between 80° C. and 90° C.
  3. temperatureafter maintaining the mixture at this temperature range for a period of between 2 and 3 hours
  4. temperaturethe reaction mixture is cooled
  5. customquenched on ice water
  6. extractionextracted with ethylacetate
  7. washwashed several times with water
  8. dry with materialAfter drying the organic solution over sodium sulfate
  9. customthe solvent is evaporated on a rotary evaporator
  10. customto obtain a very dark liquid which
  11. distillationis then distilled at 70° to 80° C.

출처 및 근거

ORD 기록
ord-89e72e5c99df4859a7416ab560b29bec
출처 데이터셋
uspto-grants-1982_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04359474

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