Tris(2-methoxyphenyl)phosphine → HCID 86711723、化合物

HRID 2285339ノート

反応式

HRID 2285339 の反応式
[N:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[C:3](B(O)O)[CH:2]=1.CCCCCCCC([C:23]([NH3+:42])([C:33]([CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH3:41])=O)C(CCCCCCC)=O)=O.[Cl-].COC1C=CC=CC=1P(C1C=CC=CC=1OC)C1C=CC=CC=1OC.O.C(=O)([O-])[O-].[Na+].[Na+].Br[C:77]1[CH:78]=[C:79]2[C:91]3=[C:92]4[C:82](=[CH:83][C:84](Br)=[CH:85][C:86]4=[CH:87][CH:88]=[C:89]3[CH:90]=1)[CH:81]=[CH:80]2>[Cl-].C([N+](CCCCCCCC)(CCCCCCCC)C)CCCCCCC.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C1(C)C=CC=CC=1>[N:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[C:3]([C:90]2[C:89]3[C:91]4=[C:92]5[C:86](=[CH:87][CH:88]=3)[CH:85]=[CH:84][C:83]([C:40]3[CH:41]=[N:42][C:23]6[C:38]([CH:39]=3)=[CH:37][CH:36]=[CH:35][CH:33]=6)=[C:82]5[CH:81]=[CH:80][C:79]4=[CH:78][CH:77]=2)[CH:2]=1

参加物

9

反応物 5

HCID 78464Tris(2-methoxyphenyl)phosphineHCID 2734663Quinoline-3-boronic acidHCID 2735133Sodium Carbonate MonohydrateHCID 136154792,7-DibromopyreneHCID 77620884Tricaprylylmethyl ammonium chloride2 回

生成物 1

HCID 86711723HCID 86711723、化合物収率 46%

試薬・触媒・溶媒 3

HCID 21218Trioctylmethylammonium chloride触媒HCID 167845palladium(II) acetate触媒HCID 1140Toluene溶媒

反応条件

温度
100 °C

実験手順

Quinoline-3-boronic acid (2.2 g, 12.2 mmol), trioctylmethylammonium chloride (trademark name: Aliquat336 (hereinafter referred to as Aliquat336), prepared by Aldrich Corporation, 0.74 g), palladium acetate (1.3 mg), tris(o-methoxyphenyl)phosphine (13.3 mg), toluene (58 ml), and sodium carbonate water solution (17.8 mmol) were added to dibromo pyrene (2.0 g, 5.6 mmol) synthesized in the prepared example and they were agitated at a temperature of 100° C. of four hours. A crystal was obtained by cooling the resultant reaction liquid at room temperature and filtering the cooled reaction (including the crystal). The compound A of 1.2 g was obtained by washing the crystal in an order of toluene, water, and methanol, and drying the washed crystal under reduced pressure (yield 46%).

後処理

  1. customA crystal was obtained
  2. temperatureby cooling the resultant
  3. customreaction liquid at room temperature
  4. filtrationfiltering
  5. customthe cooled reaction (

出典と根拠

ORDレコード
ord-787089f97ad4484e8097663416185c56
出典データセット
uspto-grants-2015_09
特許番号
US09147846B2

反応ノート

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