N,N-Dimethylaniline → 9-Chlorophenanthridine

HRID 467385ノート

反応式

HRID 467385 の反応式
P(Cl)(Cl)([Cl:3])=O.CN(C)C1C=CC=CC=1.[CH:15]1[C:28]2[C:19](=[N:20][CH:21]=[C:22]3[C:27]=2[CH:26]=[CH:25][CH:24]=[CH:23]3)[CH:18]=[CH:17][CH:16]=1>O>[Cl:3][C:25]1[CH:24]=[CH:23][C:22]2[C:27]([CH:26]=1)=[C:28]1[C:19]([CH:18]=[CH:17][CH:16]=[CH:15]1)=[N:20][CH:21]=2

参加物

5

反応物 3

HCID 949N,N-DimethylanilineHCID 9189PhenanthridineHCID 24813Phosphorus oxychloride

生成物 1

HCID 673172599-Chlorophenanthridine収率 96%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Phosphorus oxychloride (15 ml) and dimethylaniline (0.63 ml) were added to phenanthridine (2.0 g), followed by refluxing for 3 hours. The solution was poured into H2O to generate a solid, and the obtained solid was extracted with chloroform, followed by drying with sodium sulfate. After filtration, the filtrate was evaporated to dryness under reduced pressure. The obtained solid was purified by column chromatography (eluent: chloroform) (amount: 2.1 g, yield: 96%).

後処理

  1. temperatureby refluxing for 3 hours
  2. extractionthe obtained solid was extracted with chloroform
  3. dry with materialby drying with sodium sulfate
  4. filtrationAfter filtration
  5. customthe filtrate was evaporated to dryness under reduced pressure
  6. customThe obtained solid was purified by column chromatography (eluent: chloroform) (amount: 2.1 g, yield: 96%)

出典と根拠

ORDレコード
ord-efba66156385427dbe80e4808b229765
出典データセット
uspto-grants-2014_01
特許番号
US08623239B2

反応ノート

読み込み中…