Phosphorus oxychloride → 3-chloro-9-oxo-9H-indeno[1,2-b]pyrazine-2-carbonitrile

反応式

O[C:2]1[N:7]=[C:6]2[C:8]3[CH:9]=[CH:10][CH:11]=[CH:12][C:13]=3[C:14](=[O:15])[C:5]2=[N:4][C:3]=1[C:16]#[N:17].O=P(Cl)(Cl)[Cl:20]>>[Cl:20][C:2]1[N:7]=[C:6]2[C:8]3[CH:9]=[CH:10][CH:11]=[CH:12][C:13]=3[C:14](=[O:15])[C:5]2=[N:4][C:3]=1[C:16]#[N:17]

参加物

反応物 2

HCID 24813Phosphorus oxychloride

HCID 178510555HCID 178510555、化合物

生成物 1

HCID 160653593-chloro-9-oxo-9H-indeno[1,2-b]pyrazine-2-carbonitrile収率 44%

反応条件

温度: 100 °C

実験手順

A suspension of 6 (671 mg, 3.0 mmol) in POCl3 (8.4 ml) was heated under stirring to 100° C. for 17 h. Excess of POCl3 was evaporated under reduced pressure and the crude was purified by flash chromatography on silica (CH2Cl2), affording 9 (320 mg, 44%) as yellow solid.

後処理

temperaturewas heated
customExcess of POCl3 was evaporated under reduced pressure
customthe crude was purified by flash chromatography on silica (CH2Cl2)

出典と根拠

ORDレコード: ord-3ffab4eedf3a45cfb65973262b985db3
出典データセット: uspto-grants-2014_02
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08648076B2

反応ノート

読み込み中…

参加物