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Diethyl Ether → Isobutylcarbonylmethyltriphenylphosphonium bromide

HRID 1733823
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HRID 1733823 반응식
[Br:1][CH2:2][C:3]([CH2:5][CH:6]([CH3:8])[CH3:7])=[O:4].[C:9]1([P:15]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.CCOCC>C(Cl)Cl>[Br-:1].[CH2:5]([C:3]([CH2:2][P+:15]([C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1)([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1)=[O:4])[CH:6]([CH3:8])[CH3:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 11776TriphenylphosphineHCID 110844641-Bromo-4-methyl-2-pentanone

생성물 1

HCID 22914202Isobutylcarbonylmethyltriphenylphosphonium bromide수율 84.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Bromomethylisobutyl ketone (53.6 g) and triphenylphosphine (78.5 g) are intimately mixed in a 500 ml round-bottom flask and, after the initially strong heat tonality subsides, are left for 12 hours under nitrogen at room temperature. After that, the solid reaction mass is taken up in 330 ml of methylene chloride and refluxed for 30 minutes. After adding 500 ml of ether, it is allowed to cool to room temperature and the product is isolated by filtration. After drying,111.7 g of the phosphonium salt with a melting point of 244-245° C. is obtained.

후처리

  1. customAfter that, the solid reaction mass
  2. temperaturerefluxed for 30 minutes
  3. customthe product is isolated by filtration
  4. customAfter drying

출처 및 근거

ORD 기록
ord-2a5c7987061c4020a8608ccad01cf1c6
출처 데이터셋
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05532228

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