N,N-Dimethylaniline → 9-Chlorophenanthridine

HRID 467385노트

반응식

HRID 467385 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 673172599-Chlorophenanthridine수율 96%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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%).

후처리

  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%)

출처 및 근거

ORD 기록
ord-efba66156385427dbe80e4808b229765
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08623239B2

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