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

HRID 2045703

反応式

HRID 2045703 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. After 2 h, the mixture was cooled to RT; the volatiles were evaporated, and the residue was partitioned between 3M NaOH and DCM. The organic phase was dried over Na2SO4; solvent was evaporated; and the solid was 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 to reflux
  2. customthe volatiles were evaporated
  3. customthe residue was partitioned between 3M NaOH and DCM
  4. dry with materialThe organic phase was dried over Na2SO4
  5. customsolvent was evaporated
  6. customand the solid was triturated with Et2O (20 mL)
  7. filtrationfiltered

出典と根拠

ORDレコード
ord-00308b1052d444d38b285009291689d4
出典データセット
uspto-grants-2013_11
特許番号
US08591878B2

関連ノート

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