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Triphenylphosphine → HCID 86748595, 화합물

HRID 1609435
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HRID 1609435 반응식
[C:1]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=C[CH:2]=1.[F:20][C:21]1[CH:22]=[C:23]([CH:27]=[CH:28][C:29]=1[Br:30])[CH2:24][CH2:25]Br.FC1C=C(C=CC=1Br)CCO.CC(C)([O-])C.[K+].C([C:50]1([CH:56]2[CH2:61][CH2:60][CH:59]([CH2:62][CH:63]=O)[CH2:58][CH2:57]2)[CH2:55][CH2:54][CH2:53][CH2:52][CH2:51]1)C>CCOCC.C1COCC1.C1(C)C(C)=CC=CC=1>[F:20][C:21]1[CH:22]=[C:23](/[CH:24]=[CH:25]\[CH2:63][CH2:62][CH:59]2[CH2:58][CH2:57][CH:56]([CH:50]3[CH2:51][CH2:52][CH:53]([CH2:1][CH3:2])[CH2:54][CH2:55]3)[CH2:61][CH2:60]2)[CH:27]=[CH:28][C:29]=1[Br:30]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 11776TriphenylphosphineHCID 200812052-(4-Bromo-3-fluorophenyl)ethan-1-olHCID 200812081-Bromo-4-(2-bromoethyl)-2-fluorobenzeneHCID 23665647Potassium tert-butoxideHCID 54176917HCID 54176917, 화합물

생성물 1

HCID 86748595HCID 86748595, 화합물수율 42%

시약·촉매·용매 3

HCID 3283Diethyl Ether용매HCID 7237O-Xylene용매HCID 8028Tetrahydrofuran용매2회

실험 절차

Into a flask, were placed triphenylphosphine (2.9 g, 11 mmol) and 3-fluoro-4-bromophenethylbromide (2.2 g, 11 mmol) prepared from 3-fluoro-4-bromophenethylalcohol, followed by adding and dissolving xylene (15 ml), heating under reflux for 10 hours, adding THF (10 ml) to the reaction solution and stirring under ice-cooling, adding potassium-t-butoxid (1.1 g, 10 mmol) slowly to the reaction solution, stirring the reaction solution after the completion of dropping at room temperature for 2 hours, adding THF (10 ml) solution of 4-(ethylcyclohexyl) cyclohexylacetoaldehyde (2.4 g, 10 mmol), further stirring for 5 hours, adding ether after the completion of reaction, filtering off white solid deposited, concentrating the filtrate under reduced pressure, purifying the obtained brown oil by means of silica gel chromatography, to obtain a mixture (1.8 g, 4.2 mmol) of 1-(3-fluoro-4-bromophenyl)-4-(4-(4-ethylcyclohexyl)cyclohexyl)-2-Z-butene with its E-isomer.

후처리

  1. customInto a flask, were placed
  2. additionby adding
  3. temperatureheating
  4. temperatureunder reflux for 10 hours
  5. temperaturecooling
  6. stirringstirring the reaction solution after the completion
  7. stirringfurther stirring for 5 hours
  8. customafter the completion of reaction
  9. filtrationfiltering off white solid
  10. concentrationconcentrating the filtrate under reduced pressure
  11. custompurifying the obtained brown oil by means of silica gel chromatography

출처 및 근거

ORD 기록
ord-12f8f418c13b4e889771525d3b33c7bf
출처 데이터셋
uspto-grants-1995_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05401434

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