Ethanol → HCID 53868263、化合物

HRID 2396406ノート

反応式

HRID 2396406 の反応式
[CH3:1][N:2]([CH3:13])[C:3]1[CH:12]=[CH:11][C:6]([CH:7]=[CH:8][CH:9]=O)=[CH:5][CH:4]=1.[CH3:14][N:15]([CH3:33])[C:16]1[CH:21]=[CH:20][C:19]([CH:22]([C:24]2[CH:29]=[CH:28][C:27]([N:30]([CH3:32])[CH3:31])=[CH:26][CH:25]=2)[CH3:23])=[CH:18][CH:17]=1.[CH2:34](O)[CH3:35]>C(O)(=O)C>[CH3:1][N:2]([CH3:13])[C:3]1[CH:12]=[CH:11][C:6]([C:7]([C:35]2[CH:34]=[CH:21][C:16]([N:15]([CH3:33])[CH3:14])=[CH:17][CH:18]=2)=[CH:8][CH:9]([CH:23]=[C:22]([C:19]2[CH:18]=[CH:17][C:16]([N:15]([CH3:14])[CH3:33])=[CH:21][CH:20]=2)[C:24]2[CH:25]=[CH:26][C:27]([N:30]([CH3:31])[CH3:32])=[CH:28][CH:29]=2)[CH:19]=[CH:22][C:24]2[CH:29]=[CH:28][C:27]([N:30]([CH3:32])[CH3:31])=[CH:26][CH:25]=2)=[CH:5][CH:4]=1

参加物

5

反応物 3

HCID 702EthanolHCID 922244-(Dimethylamino)-cinnamaldehydeHCID 2404834,4'-ethane-1,1-diylbis(n,n-dimethylaniline)2 回

生成物 1

HCID 53868263HCID 53868263、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
5 °C

実験手順

A mixture of 5.7 g of 4-dimethylaminocinnamaldehyde, 16.2 g of 1,1-bis(4-dimethylaminophenyl)ethane, 300.0 ml of ethyl alcohol and 6.0 ml of glacial acetic acid was refluxed approximately eighteen hours. After cooling slightly an additional 3.0 g of 1,1-bis(4-dimethylaminophenyl)ethane was added and reflux maintained for an additional four hours. The resulting reaction mixture was cooled to approximately 5° C. and the solid which formed was collected by filtration. The solid was recrystallized from isopropyl alcohol, filtered and dried to obtain 16.3 g of bis{[2,2-bis(4-dimethylaminophenyl)]ethenyl}[2-(4-dimethylaminophenyl)ethenyl]methane (Formula II: R,R1,R3,R4,R9 and R10 =CH3 ; R2, R5 and R11 =H) a yellow solid which melted at 78°-82° C. Significant infrared maxims appeared at 1610 cm-1 (v.s.) and 830 cm-1 (v.s.). An acetone solution of the product spotted onto clay, phenolic resin and organic acid coated papers slowly developed a blue-colored image. Exposure of the spotted papers to bromine vapor increased the speed of color development.

後処理

  1. temperaturewas refluxed approximately eighteen hours
  2. additionwas added
  3. temperaturereflux
  4. temperaturemaintained for an additional four hours
  5. customThe resulting reaction mixture
  6. customthe solid which formed
  7. filtrationwas collected by filtration
  8. customThe solid was recrystallized from isopropyl alcohol
  9. filtrationfiltered
  10. customdried

出典と根拠

ORDレコード
ord-b8fb542f4b2b4a3a9e21a5bda896c3dc
出典データセット
uspto-grants-1996_02
特許番号
US05491262

反応ノート

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