1(2H)-Isoquinolinone → 4-Chloro-1(2H)-isoquinolone

HRID 1067241

反応式

HRID 1067241 の反応式
[Cl:1]N1C(=O)CCC1=O.[C:9]1(=[O:19])[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:12]=[CH:11][NH:10]1>C(#N)C>[Cl:1][C:12]1[C:13]2[C:18](=[CH:17][CH:16]=[CH:15][CH:14]=2)[C:9](=[O:19])[NH:10][CH:11]=1

参加物

4

反応物 2

HCID 102841(2H)-IsoquinolinoneHCID 31398Chlorosuccinimide

生成物 1

HCID 8246494-Chloro-1(2H)-isoquinolone収率 91.2%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

A solution of N-chlorosuccinimide (9.66 g, 72 mmol) in acetonitrile (MeCN) (80 mL) was added dropwise to a stirred solution of 1-(2H)-isoquinolone (10 g, 69 mmol) in MeCN (250 mL) which was being heated under reflux. The mixture was heated under reflux for an additional 1.5 h and then cooled to room temperature. The resulting precipitate was collected by filtration, with MeCN rinsing, and then dried in vacuo to give 4-chloro-1(2H)-isoquinolone (11.3 g, 62.9 mmol) as a pale pink solid.

後処理

  1. temperaturewas being heated
  2. temperatureunder reflux
  3. temperatureThe mixture was heated
  4. temperatureunder reflux for an additional 1.5 h
  5. filtrationThe resulting precipitate was collected by filtration, with MeCN rinsing
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-dbeb56870b654f5a827ced46458666ac
出典データセット
uspto-grants-2001_06
特許番号
US06248738B1

関連ノート

読み込み中…