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

반응식

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

참가 물질

반응물 2

HCID 24813Phosphorus oxychloride

HCID 178428604HCID 178428604, 화합물

생성물 1

HCID 123877362-Chloro-4-methyl-nicotinonitrile수율 89.2%

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록: ord-fd57edf38f1a444b84694a1ccd86f0ad
출처 데이터셋: uspto-grants-2000_08
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US06111112

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