Phosphorus oxychloride → Methyl 1-chloroisoquinoline-4-carboxylate

HRID 1826826ノート

反応式

HRID 1826826 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-1d307f716c314e11a2b42032ec49d8b2
出典データセット
uspto-grants-2006_05
特許番号
US07053093B2

反応ノート

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