Phosphorus oxychloride → 7-Bromo-1-chloro-6-methoxyisoquinoline

HRID 2060364

反応式

HRID 2060364 の反応式
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][NH:8][C:9]2=O)=[CH:4][C:3]=1[O:13][CH3:14].P(Cl)(Cl)([Cl:17])=O>>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][N:8]=[C:9]2[Cl:17])=[CH:4][C:3]=1[O:13][CH3:14]

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 580051257-Bromo-6-methoxy-1(2H)-isoquinolinone

生成物 1

HCID 595711467-Bromo-1-chloro-6-methoxyisoquinoline

実験手順

A mixture of the product from Step 2 (7-bromo-6-methoxyisoquinolin-1(2H)-one) (4.7 g, 18.5 mmol) in phosphorus oxychloride (30 mL) was heated to reflux for 2 h, cooled to RT, the volatiles evaporated and the residue partitioned between 3M NaOH and DCM. The organic phase was dried over Na2SO4, solvent evaporated and the solid triturated with Et2O (20 mL) and filtered to give a solid (3.75 g). LRMS ESI+ (M+H)+ 274.0.

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 2 h
  3. customthe volatiles evaporated
  4. customthe residue partitioned between 3M NaOH and DCM
  5. dry with materialThe organic phase was dried over Na2SO4, solvent
  6. customevaporated
  7. customthe solid triturated with Et2O (20 mL)
  8. filtrationfiltered

出典と根拠

ORDレコード
ord-17e8341d8d9d4154bc30772648a13051
出典データセット
uspto-grants-2012_10
特許番号
US08278322B2

関連ノート

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