ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Dimethylformamide → 4-[2-(4-Methoxyphenyl)ethenyl]-N,N-diphenylaniline

HRID 1109702
ノート
印刷プレビュー

反応式

HRID 1109702 の反応式
[C:1]1([N:7]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:8]2[CH:15]=[CH:14][C:11](C=O)=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P(=O)([O-])O[C:24](CC)([CH2:33]C)[C:25]1[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[CH:27][CH:26]=1.CN(C)C=O.C[O-].[Na+]>O.C(O)(=O)C>[C:16]1([N:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[C:8]2[CH:9]=[CH:10][C:11]([CH:33]=[CH:24][C:25]3[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[CH:27][CH:26]=3)=[CH:14][CH:15]=2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6228DimethylformamideHCID 77846Benzaldehyde, 4-(diphenylamino)-HCID 10942334Sodium MethoxideHCID 178447637HCID 178447637、化合物

生成物 1

HCID 539715084-[2-(4-Methoxyphenyl)ethenyl]-N,N-diphenylaniline収率 61.3%

試薬・触媒・溶媒 2

HCID 176
Acetic Acid
溶媒
HCID 962Water溶媒

実験手順

A mixture of 54.6 g (0.2 mol) of 4-diphenylaminobenzaldehyde, 51.6 g (0.2 mol) of diethyl-4-methoxybenzyl phosphonate, and 250 ml of dimethylformamide was placed in a 500 ml four-neck flask. 57.9 g of 28% sodium methylate was added dropwise to the above mixture with stirring at room temperature over a period of 15 minutes. Thus, the reaction was carried out at 50° to 60° C. for five hours. The thus obtained reaction mixture was diluted with 500 ml of water, and then made acid with the addition of acetic acid. Then the mixture was filtrated to obtain a wet cake. The thus obtained wet cake was washed with 100 ml of methanol three times, and recrystallized from a mixed solvent of ethanol and dioxane, whereby 46.2 g of 4-diphenylamino-4'-methoxystilbene was obtained as yellow crystals in the form of needles in a yield of 61.3%. The melting point of the obtained compound was 170° to 171.5° C.

後処理

  1. customwas placed in a 500 ml four-neck flask
  2. waitThus, the reaction was carried out at 50° to 60° C. for five hours
  3. customThe thus obtained reaction mixture
  4. filtrationThen the mixture was filtrated
  5. customto obtain a wet cake
  6. washThe thus obtained wet cake was washed with 100 ml of methanol three times
  7. customrecrystallized from a mixed solvent of ethanol and dioxane

出典と根拠

ORDレコード
ord-cdaef207c0ef4d4dad6fa2b394e5930f
出典データセット
uspto-grants-1994_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05322753

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート