Triphenylphosphine → HCID 178455762, 화합물

HRID 1600467노트

반응식

HRID 1600467 반응식
[Br:1][C:2](Br)(Br)[F:3].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[CH2:25]([C@H:27]1[CH2:32][CH2:31][C@H:30]([C@H:33]2[CH2:38][CH2:37][C@H:36]([CH:39]=O)[CH2:35][CH2:34]2)[CH2:29][CH2:28]1)[CH3:26]>COCCOC.O1CCCC1>[CH2:25]([C@H:27]1[CH2:32][CH2:31][C@H:30]([C@H:33]2[CH2:38][CH2:37][C@H:36]([CH:39]=[C:2]([F:3])[Br:1])[CH2:35][CH2:34]2)[CH2:29][CH2:28]1)[CH3:26]

참가 물질

6

반응물 3

HCID 11776TriphenylphosphineHCID 67707TribromofluoromethaneHCID 178455770HCID 178455770, 화합물

생성물 1

HCID 178455762HCID 178455762, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 80711,2-Dimethoxyethane용매

실험 절차

A solution of tribromofluoromethane and triphenyl phosphine in ethylene glycol dimethyl ether was stirred at 70° C. for 1 hour. The reaction solution was cooled with ice, and a solution of trans-4-(trans-4-ethylcyclohexyl)cyclohexane carboaldehyde in tetrahydrofuran was added thereto. After the reaction solution was further stirred for 1 hour, the temperature of the solution was gradually raised up to room temperature, and insoluble substances were removed by filtration. Dilute hydrochloric acid was added to the filtrate, and it was extracted with toluene. After the organic layer was washed with water, it was dried by using anhydrous magnesium sulfate, and concentrated under a reduced pressure to obtain a brown oily product. After this product was purified by using a silica gel column chromatography, it was recrystallized from heptane to obtain trans-4-(trans-4-ethylcyclohexyl)cyclohexyl-2-fluoro-2-bromoethene.

후처리

  1. temperatureThe reaction solution was cooled with ice
  2. customwere removed by filtration
  3. additionDilute hydrochloric acid was added to the filtrate, and it
  4. extractionwas extracted with toluene
  5. washAfter the organic layer was washed with water, it
  6. customwas dried
  7. concentrationconcentrated under a reduced pressure
  8. customto obtain a brown oily product
  9. customAfter this product was purified
  10. customwas recrystallized from heptane

출처 및 근거

ORD 기록
ord-0ef7506cc8324ddcb4daf9be46433a35
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05976408

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