1,2-Dimethoxyethane → Vinyltriphenylamine

HRID 399692

反応式

HRID 399692 の反応式
[H-].[Na+].[C:3]1([N:9]([C:16]2[CH:23]=[CH:22][C:19](C=O)=[CH:18][CH:17]=2)[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.CO[CH2:26][CH2:27]OC>[Br-].C[P+](C)(C)C.C(O)C>[CH:26]([C:17]1[CH:18]=[CH:19][CH:22]=[CH:23][C:16]=1[N:9]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1)=[CH2:27]

参加物

6

反応物 3

HCID 80711,2-DimethoxyethaneHCID 24758Sodium hydrideHCID 77846Benzaldehyde, 4-(diphenylamino)-

生成物 1

HCID 22283755Vinyltriphenylamine

試薬・触媒・溶媒 2

HCID 702Ethanol触媒HCID 357594Tetramethylphosphonium bromide触媒

実験手順

14.6 g of sodium hydride and 700 mL of 1,2-dimethoxyethane were placed in a three-neck flask, and while stirring at room temperature, 130.8 g of tetramethylphosphonium bromide was added. After adding one drop of anhydrous ethanol, the mixture was reacted for 4 hours at 70° C. Then 100 g of 4-(N,N-diphenylamino) benzaldehyde was added to the mixture. The temperature was raised to 70° C., and the mixture was reacted for 5 hours. The reaction solution was filtered, and an ether extract of the precipitate and the filtrate were washed in water. Next, the ether solution was dehydrated with calcium chloride, the ether was removed, and the reaction mixture was obtained. This was recrystallized from ethanol, and a needle-form, lemon-yellow vinyltriphenylamine was obtained. The yield was 83.4 g (yield rate of 84.0%).

後処理

  1. customthe mixture was reacted for 4 hours at 70° C
  2. temperatureThe temperature was raised to 70° C.
  3. customthe mixture was reacted for 5 hours
  4. filtrationThe reaction solution was filtered
  5. extractionan ether extract of the precipitate
  6. washthe filtrate were washed in water
  7. customthe ether was removed
  8. customthe reaction mixture was obtained
  9. customThis was recrystallized from ethanol

出典と根拠

ORDレコード
ord-c7721db1cd6043c1bc0e09126b620871
出典データセット
uspto-grants-1998_10
特許番号
US05824443

関連ノート

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