Hydroxyamine hydrochloride → 2-Chloroquinoline-3-carbonitrile

HRID 2413152

反応式

HRID 2413152 の反応式
[Cl:1][C:2]1[C:11]([CH:12]=O)=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.Cl.[NH2:15]O>P(Cl)(Cl)(Cl)=O>[Cl:1][C:2]1[C:11]([C:12]#[N:15])=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 6909582-Chloro-3-quinolinecarboxaldehyde

生成物 1

HCID 115646012-Chloroquinoline-3-carbonitrile収率 71.1%

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

実験手順

A mixture was prepared from 10 g of 2-chloro-3-quinolinecarboxaldehyde, 5.2 g of hydroxylamine hydrochloride and 100 ml of phosphoryl chloride and heated with a heat lamp. The mixture was heterogeneous until the temperature reached 90° C. and there was no noticeable exotherm or gas evolution. After heating at reflux for 30 minutes, the mixture was cooled for 16 hours. It was then quenched in 700 ml of water. The tan solid which formed was separated by filtration and dried to give 7 g of crude 2-chloro-3-cyanoquinoline.

後処理

  1. temperatureheated with a heat lamp
  2. customreached 90° C.
  3. temperatureAfter heating
  4. temperatureat reflux for 30 minutes
  5. temperaturethe mixture was cooled for 16 hours
  6. customIt was then quenched in 700 ml of water
  7. customThe tan solid which formed
  8. customwas separated by filtration
  9. customdried

出典と根拠

ORDレコード
ord-8445ec0f90394645a7e7b4ce05565a26
出典データセット
uspto-grants-1985_01
特許番号
US04496569

関連ノート

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