1,2-Dimethoxyethane → HCID 86660754、化合物

HRID 1404886ノート

反応式

HRID 1404886 の反応式
Br[C:2]1[C:15]2[C:16]3=[C:17]4[C:12](=[CH:13][CH:14]=2)[CH:11]=[C:10]([C:18]([CH3:21])([CH3:20])[CH3:19])[CH:9]=[C:8]4[CH:7]=[CH:6][C:5]3=[C:4](Br)[CH:3]=1.[Cl:23][C:24]1[CH:29]=[CH:28][C:27](B(O)O)=[CH:26][CH:25]=1.C(=O)([O-])[O-].[Na+].[Na+].CO[CH2:41][CH2:42]OC>Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.O>[C:18]([C:10]1[CH:11]=[C:12]2[C:17]3=[C:16]4[C:15](=[C:2]([C:42]5[CH:41]=[CH:29][C:24]([Cl:23])=[CH:25][CH:26]=5)[CH:3]=[C:4]([C:27]5[CH:28]=[CH:29][C:24]([Cl:23])=[CH:25][CH:26]=5)[C:5]4=[CH:6][CH:7]=[C:8]3[CH:9]=1)[CH:14]=[CH:13]2)([CH3:19])([CH3:21])[CH3:20]

参加物

7

反応物 4

HCID 80711,2-DimethoxyethaneHCID 10340Sodium CarbonateHCID 742994-Chlorophenylboronic acidHCID 579534681,3-Dibromo-7-tert-butylpyrene

生成物 1

HCID 86660754HCID 86660754、化合物

試薬・触媒・溶媒 2

HCID 178418476HCID 178418476、化合物触媒HCID 962Water溶媒

反応条件

温度
5 °C

実験手順

Then, a mixed solution of 20.0 g of 1,3-dibromo-7-t-butylpyrene, 16.52 g of 4-chlorophenylboronic acid, 0.034 g of bis(triphenylphosphine)dichloropalladium, 106 ml of an aqueous 2M sodium carbonate solution and 240 ml of 1,2-dimethoxyethane was heated and stirred for about 5 hours under a nitrogen stream and under refluxing, and this was cooled to 5° C. After 240 ml of water was added, and the precipitated solid was filtered, the solid was washed with 125 ml of water two times and 125 ml of methanol once. After the solid was vacuum dried, the gray solid was dissolved in 48 ml of toluene, 2 g of active carbon was added, this was stirred for about 15 minutes, and the active carbon was filtered. After the resulting filtrate was evaporated, 100 ml of hexane was added, and the mixture was stirred for about 1 hour, and filtered. After the resultant was vacuum dried, 7.7 g of 7-t-butyl-1,3-bis(4-chlorophenyl)pyrene was obtained.

後処理

  1. temperatureunder refluxing
  2. filtrationthe precipitated solid was filtered
  3. washthe solid was washed with 125 ml of water two times and 125 ml of methanol once
  4. customdried
  5. dissolutionthe gray solid was dissolved in 48 ml of toluene
  6. addition2 g of active carbon was added
  7. stirringthis was stirred for about 15 minutes
  8. filtrationthe active carbon was filtered
  9. customAfter the resulting filtrate was evaporated
  10. addition100 ml of hexane was added
  11. stirringthe mixture was stirred for about 1 hour
  12. filtrationfiltered
  13. customdried

出典と根拠

ORDレコード
ord-7a6255ddf7bd41c0ac9f31bf89df5764
出典データセット
uspto-grants-2014_12
特許番号
US08916275B2

反応ノート

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