Phosphorus oxychloride → 4-Chloro-3-(2-chloroethyl)cinnoline

HRID 704567

反応式

HRID 704567 の反応式
[Cl:1][CH2:2][CH2:3][C:4]1[C:13](=O)[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[NH:6][N:5]=1.P(Cl)(Cl)([Cl:17])=O>>[Cl:1][CH2:2][CH2:3][C:4]1[N:5]=[N:6][C:7]2[C:12]([C:13]=1[Cl:17])=[CH:11][CH:10]=[CH:9][CH:8]=2

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 200727583-(2-Chloroethyl)-4-oxo-(1H)-cinnoline

生成物 1

HCID 200727524-Chloro-3-(2-chloroethyl)cinnoline

実験手順

3-(2-Chloroethyl)-4-oxo-(1H)-cinnoline (9 g, 0.043 mol) and phosphorus oxychloride (90 ml) were heated under reflux for 1 hour. After allowing to cool, the excess phosphorus oxychloride was evaporated under reduced pressure and the residue was poured onto ice (100 g), basified with concentrated ammonia solution, and extracted with chloroform (3×100 ml). The chloroform extracts were combined, dried over magnesium sulphate and evaporated under reduced pressure to give a solid, 8.00 g. Recrystallization from diethyl ether gave the title compound, m.p. 81-82°.

後処理

  1. temperatureunder reflux for 1 hour
  2. temperatureto cool
  3. customthe excess phosphorus oxychloride was evaporated under reduced pressure
  4. additionthe residue was poured onto ice (100 g)
  5. extractionextracted with chloroform (3×100 ml)
  6. dry with materialdried over magnesium sulphate
  7. customevaporated under reduced pressure
  8. customto give a solid, 8.00 g
  9. customRecrystallization from diethyl ether

出典と根拠

ORDレコード
ord-d075416f26954eb8b0f827581e8b9a58
出典データセット
uspto-grants-1991_01
特許番号
US04988695

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