Phosphorus oxychloride → HCID 21578662、化合物

反応式

[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[NH:8][C:7](=O)[CH:6]=[C:5]2[C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[CH:14]=1.P(Cl)(Cl)([Cl:22])=O>>[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([Cl:22])[CH:6]=[C:5]2[C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[CH:14]=1

参加物

反応物 2

HCID 24813Phosphorus oxychloride

HCID 12016671HCID 12016671、化合物

生成物 1

HCID 21578662HCID 21578662、化合物収率 100%

実験手順

A mixture of intermediate (4) (0.16 mol) in phosphoryl chloride (500 ml) was stirred and refluxed for one night. The mixture was evaporated till dryness, the residue was taken up in ice and water, alkalized with NH4OH and extracted with DCM. The organic layer was decanted, dried (MgSO4), filtered off and evaporated, yielding 56 g (100%) 6-bromo-2-chloro-4-(3-chlorophenyl)quinoline, mp. 125° C. (intermediate 5).

後処理

temperaturerefluxed for one night
customThe mixture was evaporated till dryness
extractionextracted with DCM
customThe organic layer was decanted
dry with materialdried (MgSO4)
filtrationfiltered off
customevaporated

出典と根拠

ORDレコード: ord-9b4dc5a241b04126ad43a26ab7064a83
出典データセット: uspto-grants-2006_06
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US07067531B2

反応ノート

読み込み中…

参加物