Phosphorus oxychloride → 1-Chloro-6-methoxy-3-methylisoquinoline

HRID 1511472ノート

反応式

HRID 1511472 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9](=O)[NH:8][C:7]([CH3:14])=[CH:6]2.P(Cl)(Cl)([Cl:17])=O>>[Cl:17][C:9]1[C:10]2[C:5](=[CH:4][C:3]([O:2][CH3:1])=[CH:12][CH:11]=2)[CH:6]=[C:7]([CH3:14])[N:8]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 123270606-Methoxy-3-methylisoquinolin-1(2H)-one

生成物 1

HCID 578930951-Chloro-6-methoxy-3-methylisoquinoline

実験手順

The isoquinoline of step 2 was dissolved in phosphorus oxychloride (2.5 mL) and heated at reflux for 1 hour. The excess phosphorus oxychloride was removed under reduced pressure and the residue was dissolved in chloroform. The resulting solution was washed with 1N aq. sodium hydroxide, water and brine. Evaporation of the solvent under reduced pressure gave crude 1-chloro-6-methoxy-3-methylisoquinoline, which was used directly in the next step.

後処理

  1. temperatureheated
  2. temperatureat reflux for 1 hour
  3. customThe excess phosphorus oxychloride was removed under reduced pressure
  4. dissolutionthe residue was dissolved in chloroform
  5. washThe resulting solution was washed with 1N aq. sodium hydroxide, water and brine
  6. customEvaporation of the solvent under reduced pressure

出典と根拠

ORDレコード
ord-04e0c1e65adf462e83c139abb7ab8e91
出典データセット
uspto-grants-2012_07
特許番号
US08211897B2

反応ノート

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