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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Triphenylphosphine → HCID 58592758, 화합물

HRID 642851
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HRID 642851 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[C:9]([F:12])([F:11])[F:10])=[CH:4][CH:3]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.Cl[C:34]([F:39])([F:38])C([O-])=O.[Na+].[F-:41].[K+]>COCCOCCOC.O>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:34]([F:39])([F:41])[F:38])[C:9]([F:12])([F:11])[F:10])=[CH:4][CH:3]=1
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7

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HCID 11776TriphenylphosphineHCID 522689Potassium FluorideHCID 6038664'-Bromo-2,2,2-trifluoroacetophenoneHCID 2734985Sodium chlorodifluoroacetate

생성물 1

HCID 58592758HCID 58592758, 화합물

시약·촉매·용매 2

HCID 962Water용매2회
HCID 8150
Diglyme
용매
2회

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온도
150 °C

실험 절차

1-(4-Bromo-phenyl)-2,2,2-trifluoro-ethanone (500 mg, 2 mmol) and triphenylphosphine (1.05 g, 4 mmol) were dissolved in diglyme (25 ml) and heated to 150° C. in a three-neck flask fitted with both an addition funnel and a reflux condenser under nitrogen. A solution of sodium chlorodifluoroacetate, dissolved in diglyme (13 ml), was slowly added via the addition funnel. The addition took about one hour. After it was complete, the reaction mixture was allowed to stir for an additional hour. It was then cooled to below 100° C., and potassium fluoride (476 mg, 8.2 mmol) and water (0.3 ml) were added. The mixture was allowed to stir for 18 h at 95° C. The reaction mixture was heated to 130° C., water was added and the title product was steam distilled into a collection flask (with a large amount of diglyme, complicating yield calculations). 1H NMR (CDCl3) δ=7.61 (d, J=8.4 Hz, 2H), 7.32 (d, J=8.4 Hz, 2H), 4.06 (septet, JH,F=8.2 Hz, 1H).

후처리

  1. customfitted with both an addition funnel and a reflux condenser under nitrogen
  2. additionwas slowly added via the addition funnel
  3. additionThe addition
  4. temperatureIt was then cooled to below 100° C.
  5. stirringto stir for 18 h at 95° C
  6. temperatureThe reaction mixture was heated to 130° C.

출처 및 근거

ORD 기록
ord-6296cfb5da8e49f3812f18d43b7e5695
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07696210B2

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