Sodium Hydroxide → 7-Bromo-1,3-dichloroisoquinoline

HRID 2060367ノート

反応式

HRID 2060367 の反応式
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][N+:8]([O-])=[C:9]2[Cl:12])=[CH:4][CH:3]=1.[OH-].[Na+].O=P(Cl)(Cl)[Cl:18]>>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[C:7]([Cl:18])[N:8]=[C:9]2[Cl:12])=[CH:4][CH:3]=1

参加物

4

反応物 3

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 581282867-Bromo-1-chloroisoquinoline 2-oxide

生成物 1

HCID 534012027-Bromo-1,3-dichloroisoquinoline

実験手順

7-Bromo-1-chloroisoquinoline 2-oxide (1.43 g, 5.56 mmol) and POCl3 (20 mL) were heated at reflux for 2 h. The reaction mixture was cooled and carefully poured onto a mixture of ice/water (500 g), stirred for 1 h and the pH adjusted to 10.0 with 10M NaOH. The mixture was extracted with chloroform (2×100 mL) and the chloroform extracts washed with brine, dried over MgSO4, filtered and concentrated to give the title compound (1.40 g). LRMS (M+H)+=276.0.

後処理

  1. temperatureat reflux for 2 h
  2. temperatureThe reaction mixture was cooled
  3. extractionThe mixture was extracted with chloroform (2×100 mL)
  4. washthe chloroform extracts washed with brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-dd328fa39e7542539dd613b5fa2c0f81
出典データセット
uspto-grants-2012_10
特許番号
US08278322B2

反応ノート

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