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Triphenylphosphine → HCID 67923954, 화합물

HRID 973867
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HRID 973867 반응식
[Br:1]C1OCC=C1.[CH3:7][C:8]1[CH:9]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:10](=[O:13])[O:11][CH:12]=1.[C:20]1([P:26]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>C1C=CC=CC=1>[Br-:1].[CH3:7][C:8]1[CH:9]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:10](=[O:13])[O:11][C:12]=1[P+:26]([C:27]1[CH2:32][CH:31]=[CH:30][CH2:29][CH:28]=1)([C:33]1[CH2:34][CH:35]=[CH:36][CH2:37][CH:38]=1)[C:20]1[CH2:25][CH:24]=[CH:23][CH2:22][CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 11776TriphenylphosphineHCID 67923942HCID 67923942, 화합물

생성물 1

HCID 67923954HCID 67923954, 화합물수율 109.8%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

5-Bromo-2,5-dihydrofuran-4-methyl-2-oxo-3-phenylfuran (3.46 g) and triphenylphosphine (4.14 g) in benzene (50 mls), were heated under reflux overnight. The colourless salt was filtered off, washed with benzene, then ether (2 portions), and dried to give the title compound as a white solid, (6.13 g, 85%), m.p. 214°-217° C. (decomp), acetonitrile/ethyl acetate. (Found: C, 67.21; H, 4.61; Br, 15.65%. C29H24BrO2P requires C, 67.58; H, 4.69; Br, 15.51%); νmax (CH2Cl2) 1775(s)cm-1 ; δH (CDCl3) 2.14 (3H,d,J4Hz), 7.1-8.5 (20H,m) and 9.75 (1H,d,J7Hz); [mass spectrum: +ve ion (thioglycerol) MH+, 435].

후처리

  1. temperatureunder reflux overnight
  2. filtrationThe colourless salt was filtered off
  3. washwashed with benzene
  4. dry with materialether (2 portions), and dried

출처 및 근거

ORD 기록
ord-71eadb77ff274d28907964278c56866a
출처 데이터셋
uspto-grants-1991_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05064649

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