Phosphorus oxychloride → HCID 22341136、化合物

HRID 584682ノート

反応式

HRID 584682 の反応式
[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

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 22341064HCID 22341064、化合物

生成物 1

HCID 22341136HCID 22341136、化合物収率 21%

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-2e3627308cef4a78801d6d5207f35d54
出典データセット
uspto-grants-2005_08
特許番号
US06927214B1

反応ノート

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