Phosphorus oxychloride → 4-Chloro-3-(2-chloroethyl)-8-methylcinnoline

HRID 704571

反応式

HRID 704571 の反応式
[Cl:1][CH2:2][CH2:3][C:4]1[C:13](=O)[C:12]2[C:7](=[C:8]([CH3:15])[CH:9]=[CH:10][CH:11]=2)[NH:6][N:5]=1.P(Cl)(Cl)([Cl:18])=O>>[Cl:1][CH2:2][CH2:3][C:4]1[N:5]=[N:6][C:7]2[C:12]([C:13]=1[Cl:18])=[CH:11][CH:10]=[CH:9][C:8]=2[CH3:15]

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 200727593-(2-Chloroethyl)-8-methyl-4(1H)-cinnolinone

生成物 1

HCID 200727624-Chloro-3-(2-chloroethyl)-8-methylcinnoline

実験手順

3-(2-Chloroethyl)-8-methyl-4-oxo-(1H)-cinnoline (9 g, 0.04 mol) and phosphorus oxychloride (100 ml) were heated under reflux for 2 hours. The excess phosphorus oxychloride was evaporated under reduced pressure and the residue was poured onto ice, basified with concentrated ammonia solution and extracted with chloroform (3×200 ml). The chloroform extracts were combined, dried over magnesium sulphate, filtered and evaporated under reduced pressure to give a dark brown solid. Recrystallization from diethyl ether/petroleum ether (b.p. 40-60°) gave an analytically pure sample, m.p. 102-104°

後処理

  1. temperatureunder reflux for 2 hours
  2. customThe excess phosphorus oxychloride was evaporated under reduced pressure
  3. additionthe residue was poured onto ice
  4. extractionextracted with chloroform (3×200 ml)
  5. dry with materialdried over magnesium sulphate
  6. filtrationfiltered
  7. customevaporated under reduced pressure
  8. customto give a dark brown solid
  9. customRecrystallization from diethyl ether/petroleum ether (b.p. 40-60°)
  10. customgave an analytically pure sample, m.p. 102-104°

出典と根拠

ORDレコード
ord-bd35c621611c4b6da795f39f32d439a6
出典データセット
uspto-grants-1991_01
特許番号
US04988695

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