Phosphorus oxychloride → 2-Chloro-5,6-dimethylpyridine-3-carbonitrile

反応式

P(Cl)(Cl)([Cl:3])=O.O=[C:7]1[C:12]([C:13]#[N:14])=[CH:11][C:10]([CH3:15])=[C:9]([CH3:16])[NH:8]1>>[Cl:3][C:7]1[C:12]([C:13]#[N:14])=[CH:11][C:10]([CH3:15])=[C:9]([CH3:16])[N:8]=1

参加物

反応物 2

HCID 24813Phosphorus oxychloride

HCID 5905325,6-Dimethyl-2-oxo-1,2-dihydropyridine-3-carbonitrile

生成物 1

HCID 128911062-Chloro-5,6-dimethylpyridine-3-carbonitrile収率 66.7%

実験手順

Phosphorus oxychloride (15 mL) was added to 2-oxo-1,2-dihydro-5,6-dimethyl pyridine-3-carbonitrile (2.00 g, 13.5 mmol) in a two neck 50 mL round bottom flask, and this mixture was stirred at RT for 1 h, and then refluxed for 12 h. Afterwards, the excess phosphorous oxychloride was distilled off, and the residue was poured into ice cooled water. The aqueous solution was basified with saturated sodium bicarbonate solution, and the precipitate that formed was filtered off to afford the title compound (1.50 g), yield: 66.7%.

後処理

temperaturerefluxed for 12 h
distillationAfterwards, the excess phosphorous oxychloride was distilled off
additionthe residue was poured into ice
temperaturecooled water
customthe precipitate that formed
filtrationwas filtered off

出典と根拠

ORDレコード: ord-b309e95cbe9f4594af1d5931b4a3cb26
出典データセット: uspto-grants-2015_05
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09040558B2

反応ノート

読み込み中…

参加物