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Triphenylphosphine → HCID 86748595、化合物

HRID 1609435
ノート
印刷プレビュー

反応式

HRID 1609435 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

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

生成物 1

HCID 86748595HCID 86748595、化合物収率 42%

試薬・触媒・溶媒 3

HCID 3283Diethyl Ether溶媒HCID 7237O-Xylene溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-12f8f418c13b4e889771525d3b33c7bf
出典データセット
uspto-grants-1995_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05401434

反応ノート

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