Phosphorus oxychloride → 4-Chloro-6-nitroquinoline-3-carbonitrile

HRID 379107

反応式

HRID 379107 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[NH:10][CH:9]=[C:8]([C:14]#[N:15])[C:7]2=O)([O-:3])=[O:2].P(Cl)(Cl)([Cl:19])=O>>[Cl:19][C:7]1[C:6]2[C:11](=[CH:12][CH:13]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=2)[N:10]=[CH:9][C:8]=1[C:14]#[N:15]

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 110530426-Nitro-4-oxo-1,4-dihydroquinoline-3-carbonitrile

生成物 1

HCID 110856904-Chloro-6-nitroquinoline-3-carbonitrile

実験手順

A mixture of 31.3 g (0.147 mol) of 6-nitro-4-oxo-1,4-dihydro-quinoline-3-carbonitrile and 160 mL of phosphorous oxychloride was refluxed for 5.5 h. The phosphorous oxychloride was removed in vacuo and the residue was poured over ice and neutralized with sodium bicarbonate. The product was collected, washed with water and dried in vacuo (50° C.). There was obtained 33.5 g of tan solid; solid: mass spectrum (electrospray, m/e): M+H 234.

後処理

  1. temperaturewas refluxed for 5.5 h
  2. customThe phosphorous oxychloride was removed in vacuo
  3. additionthe residue was poured over ice and neutralized with sodium bicarbonate
  4. customThe product was collected
  5. washwashed with water
  6. customdried in vacuo (50° C.)

出典と根拠

ORDレコード
ord-76f319dff7ae4a3e86716aa3e7b3e0be
出典データセット
uspto-grants-2001_10
特許番号
US06297258B1

関連ノート

読み込み中…