Phosphorus oxychloride → 2-Chloro-4-methyl-nicotinonitrile

反応式

O[C:2]1[C:7]([C:8]#[N:9])=[C:6]([CH3:10])[CH:5]=[CH:4][N:3]=1.P(Cl)(Cl)([Cl:13])=O>>[Cl:13][C:2]1[C:7]([C:8]#[N:9])=[C:6]([CH3:10])[CH:5]=[CH:4][N:3]=1

参加物

反応物 2

HCID 24813Phosphorus oxychloride

HCID 178428604HCID 178428604、化合物

生成物 1

HCID 123877362-Chloro-4-methyl-nicotinonitrile収率 89.2%

実験手順

To a 250 mL flask equipped with a magnetic stirrer was added 10 g of 2-hydroxy-4-methyl-3-pyridinylcarbonitrile (8) and 60 mL of phosphorous oxychloride. The mixture was refluxed for one hour. The excess POCl3 was distilled under reduced pressure. The residue was poured into water. The crystalline material was filtered and dried at to give 10.2 g (89.2%) of (9). m.p.: 109-110° C., NMR (DMSO); ppm: 2.56 (s,3H); 7.6 (bs,1H); 8.56 (m,1H).

後処理

customTo a 250 mL flask equipped with a magnetic stirrer
temperatureThe mixture was refluxed for one hour
distillationThe excess POCl3 was distilled under reduced pressure
additionThe residue was poured into water
filtrationThe crystalline material was filtered
customdried at

出典と根拠

ORDレコード: ord-fd57edf38f1a444b84694a1ccd86f0ad
出典データセット: uspto-grants-2000_08
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US06111112

反応ノート

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参加物