1,2-Dimethoxyethane → Vinyltriphenylamine

HRID 727429

反応式

HRID 727429 の反応式
[H-].[Na+].CO[CH2:5][CH2:6]OC.[C:9]1([N:15]([C:22]2[CH:29]=[CH:28][C:25](C=O)=[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>[Br-].C[P+](C)(C)C.C(O)C>[CH:5]([C:23]1[CH:24]=[CH:25][CH:28]=[CH:29][C:22]=1[N:15]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=[CH2:6]

参加物

7

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 3

HCID 702Ethanol触媒HCID 357594Tetramethylphosphonium bromide触媒HCID 702Ethanol溶媒

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, the temperature was raised to 70° C., and the mixture was reacted for 5 hours. The 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 crude product was obtained. Vinyltriphenylamine was obtained as lemon yellow needles upon recrystalization from ethanol. The yield was 83.4 g (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 solution was filtered
  5. extractionan ether extract of the precipitate
  6. washthe filtrate were washed in water
  7. customthe ether was removed
  8. customthe crude product was obtained

出典と根拠

ORDレコード
ord-81fb856ce0ad449e94febb5b56fea5b1
出典データセット
uspto-grants-1998_01
特許番号
US05712360

関連ノート

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