Potassium Carbonate → HCID 23042045, 화합물

HRID 2166092노트

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HRID 2166092 반응식
C(=O)([O-])[O-].[K+].[K+].Cl.[F:8][C:9]([F:19])([F:18])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[NH:16][NH2:17].[F:20][C:21]1[CH:29]=[CH:28][CH:27]=[C:26]([F:30])[C:22]=1[C:23](F)=[O:24].[OH-].[Ca+2].[OH-]>O.C(OCC)(=O)C>[F:20][C:21]1[CH:29]=[CH:28][CH:27]=[C:26]([F:30])[C:22]=1[C:23]([NH:17][NH:16][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=1[C:9]([F:18])([F:19])[F:8])=[O:24]

참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 6093208Calcium HydroxideHCID 12891828[2-(Trifluoromethyl)phenyl]hydrazine--hydrogen chloride (1/1)HCID 217311632,6-Difluorobenzoyl fluoride

생성물 1

HCID 23042045HCID 23042045, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

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온도
3 °C

실험 절차

13.6 g (98 mmol) of potassium carbonate in 70 ml of water are added at 10° C. while stirring to a suspension of 10.4 g (49 mmol) of α,α,α-trifluoro-o-tolylhydrazine hydrochloride in 50 ml of ethyl acetate. 7.8 g (49 mmol) of 2,6-difluorobenzoyl fluoride are subsequently added dropwise to the clear solution while cooling so that the internal temperature is maintained at 3° C. The mixture is stirred at 5° C. for 60 minutes and thereafter at 25° C. for 4 hours, and the organic phase is separated. The aqueous phase is back-extracted with 50 ml of ethyl acetate and subsequently treated with 1.85 g (25 mmol) of calcium hydroxide in order to precipitate the calcium fluoride. The combined organic phases are washed in each case once with dilute hydrochloric acid and sodium bicarbonate solution, dried over anhydrous magnesium sulfate and evaporated under reduced pressure. After recrystallization from acetone and n-hexane there is obtained 2,6-difluoro-N' -(α,α,α-trifluoro-o-tolyl)-benzhydrazide as a white crystallizate, m.p. 129°-130° C.; mass spectrum m/e: M+ 316(26), 141(100).

후처리

  1. temperaturewhile cooling so that the internal temperature
  2. waitat 25° C. for 4 hours
  3. customthe organic phase is separated
  4. extractionThe aqueous phase is back-extracted with 50 ml of ethyl acetate
  5. customto precipitate the calcium fluoride
  6. washThe combined organic phases are washed in each case once with dilute hydrochloric acid and sodium bicarbonate solution
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customevaporated under reduced pressure
  9. customAfter recrystallization from acetone and n-hexane

출처 및 근거

ORD 기록
ord-188253962fee4288829418d5ae86ee68
출처 데이터셋
uspto-grants-1990_07
특허 번호
US04943583

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