Phosphorus oxychloride → 1-Chloro-6-methoxyisoquinoline

HRID 719838ノート

反応式

HRID 719838 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][CH:7]=[CH:6]2.O=P(Cl)(Cl)[Cl:16]>>[Cl:16][C:9]1[C:10]2[C:5](=[CH:4][C:3]([O:2][CH3:1])=[CH:12][CH:11]=2)[CH:6]=[CH:7][N:8]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 218898546-methoxyisoquinolin-1(2H)-one

生成物 1

HCID 219010741-Chloro-6-methoxyisoquinoline

実験手順

6-Methoxy-2H-isoquinolin-1-one in POCl3 was heated to gentle reflux for 3 h then evaporated in vacuo. The residue was poured into ice-water (20 mL) and neutralized to pH 10 with 10 M NaOH. Extracted with CHCl3. The organic layer was washed with brine, dried over MgSO4, filtered, evaporated. The residue was purified by flash chromatography (hexane-EtOAc) to afford a white solid.

後処理

  1. temperatureto gentle reflux for 3 h
  2. customthen evaporated in vacuo
  3. additionThe residue was poured into ice-water (20 mL)
  4. extractionExtracted with CHCl3
  5. washThe organic layer was washed with brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue was purified by flash chromatography (hexane-EtOAc)
  10. customto afford a white solid

出典と根拠

ORDレコード
ord-731a4ab402a44243ba25b206546e7f7b
出典データセット
uspto-grants-2006_11
特許番号
US07132504B2

反応ノート

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