Phosphorus oxychloride → Methyl 1-chloroisoquinoline-4-carboxylate

HRID 1635913ノート

反応式

HRID 1635913 の反応式
O=[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([C:12]([O:14][CH3:15])=[O:13])=[CH:4][NH:3]1.O=P(Cl)(Cl)[Cl:18]>>[Cl:18][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([C:12]([O:14][CH3:15])=[O:13])=[CH:4][N:3]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 641184Methyl 1-Oxo-2H-Isoquinoline-4-Carboxylate

生成物 1

HCID 3338790Methyl 1-chloroisoquinoline-4-carboxylate

反応条件

温度
100 °C

実験手順

A mixture of the product from part 3 (12.5 g) in 50 ml of POCl3 is stirred at 100° C. for about two hours then cooled and concentrated under vacuum. The residue is dissolved in 300 ml of CHCl3, and the resulting solution is washed with aqueous NaHCO3 and water, dried over Na2SO4, filtered and then concentrated to give the title compound, m.p. 53-55° C.

後処理

  1. temperaturethen cooled
  2. concentrationconcentrated under vacuum
  3. dissolutionThe residue is dissolved in 300 ml of CHCl3
  4. washthe resulting solution is washed with aqueous NaHCO3 and water
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-3f0aceb3214a48b4a5201288d74ad72e
出典データセット
uspto-grants-2003_01
特許番号
US06511987B1

反応ノート

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