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Ethylene Glycol → (2-Hydroxyphenyl)tris(4-methoxyphenyl)phosphanium bromide

HRID 1686854
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인쇄 미리보기

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HRID 1686854 반응식
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[OH:8].[CH3:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([P:17]([C:26]2[CH:31]=[CH:30][C:29]([O:32][CH3:33])=[CH:28][CH:27]=2)[C:18]2[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=2)=[CH:13][CH:12]=1.C(O)CO>[Ni](Cl)Cl.O>[Br-:1].[CH3:25][O:24][C:21]1[CH:22]=[CH:23][C:18]([P+:17]([C:26]2[CH:27]=[CH:28][C:29]([O:32][CH3:33])=[CH:30][CH:31]=2)([C:14]2[CH:15]=[CH:16][C:11]([O:10][CH3:9])=[CH:12][CH:13]=2)[C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=2[OH:8])=[CH:19][CH:20]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 174Ethylene GlycolHCID 72442-BromophenolHCID 70071Phosphine, tris(4-methoxyphenyl)-

생성물 1

HCID 71403132(2-Hydroxyphenyl)tris(4-methoxyphenyl)phosphanium bromide

시약·촉매·용매 2

HCID 24385Nickel Dichloride촉매HCID 962Water용매

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온도
160 °C

실험 절차

10.4 g (0.060 mol) of 2-bromophenol, 23.20 g (0.066 mol) of tris(4-methoxyphenyl) phosphine, 0.65 g (5 mmol) of nickel chloride, and 40 ml of ethylene glycol were put into a separable flask (volume, 200 ml) equipped with a condenser and a stirrer, and reacted with stirring under heat at 160° C. The reaction liquid was cooled, 40 ml of pure water was dropwise added thereto, and the deposited crystal was washed with toluene, taken out through filtration, and dried to obtain tris(4-methoxyphenyl)(2-hydroxyphenyl)phosphonium bromide.

후처리

  1. custom(volume, 200 ml) equipped with a condenser and a stirrer
  2. customreacted
  3. customThe reaction liquid
  4. temperaturewas cooled
  5. washthe deposited crystal was washed with toluene
  6. filtrationtaken out through filtration
  7. customdried

출처 및 근거

ORD 기록
ord-a028361eb6cd40cd9192dc7287c710cd
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08148831B2

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