Phosphorus oxychloride → HCID 22341136, 화합물

HRID 584682노트

반응식

HRID 584682 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[Cl:12])[NH:8][C:7](=O)[C:6]([CH2:14][CH2:15][CH2:16][Cl:17])=[N:5]2.O=P(Cl)(Cl)[Cl:20]>>[Cl:20][C:7]1[C:6]([CH2:14][CH2:15][CH2:16][Cl:17])=[N:5][C:4]2[C:9](=[CH:10][C:11]([Cl:12])=[C:2]([Cl:1])[CH:3]=2)[N:8]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 22341064HCID 22341064, 화합물

생성물 1

HCID 22341136HCID 22341136, 화합물수율 21%

실험 절차

6,7-Dichloro-3-(3-chloropropyl)-1H-quinoxalin-2-one (0.68 g, 2.33 mmol) was added to POCl3 (10 ml) and the resulting mixture was heated under reflux for 0.5 hours. The reaction mixture was poured onto ice and extracted with dichloromethane (3×). The combined organic layers were dried over anhydrous sodium sulfate, filtered and evaporate in vacuo. The resulting oil was purified by flash column chromatography (dichloromethane) to yield 21% of 2,6,7-trichloro-3-(3-chloropropyl)quinoxaline as a colourless oil.

후처리

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 0.5 hours
  3. additionThe reaction mixture was poured onto ice
  4. extractionextracted with dichloromethane (3×)
  5. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. customevaporate in vacuo
  8. customThe resulting oil was purified by flash column chromatography (dichloromethane)

출처 및 근거

ORD 기록
ord-2e3627308cef4a78801d6d5207f35d54
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06927214B1

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