Dimethylformamide → HCID 178429078、化合物

反応式

[Cl:1][C:2]1[N:9]=[C:8]([CH3:10])[CH:7]=[C:6](Cl)[C:3]=1[C:4]#[N:5].CN(C)C=[O:15]>>[Cl:1][C:2]1[N:9]=[C:8]([CH3:10])[CH:7]=[C:6]([OH:15])[C:3]=1[C:4]#[N:5]

参加物

反応物 2

HCID 6228Dimethylformamide

HCID 112754712,4-Dichloro-6-methylnicotinonitrile

生成物 1

HCID 178429078HCID 178429078、化合物収率 84.1%

反応条件

温度: 80 °C

実験手順

A mixture of 2,4-dichloro-6-methylnicotinonitrile (12.0 g, 64.2 mmol), CsOAc (37.0 g, 193.0 mmol) in N,N-dimethylformamide (50 mL) was stirred at 80° C. overnight under N2. The mixture was partitioned between water (800 mL) and ethyl acetate (800 mL), the organic layer was dried and concentrated to afford 2-chloro-4-hydroxy-6-methylnicotinonitrile (9.0 g brown solid, 84.1% yield).

後処理

customThe mixture was partitioned between water (800 mL) and ethyl acetate (800 mL)
customthe organic layer was dried
concentrationconcentrated

出典と根拠

ORDレコード: ord-3720d08b320a4fcfadb223f723a7f49d
出典データセット: uspto-grants-2016_06
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09371331B2

反応ノート

読み込み中…

参加物