Phosphorus oxychloride → 7-Chloro-1-(difluoromethyl)-8-phenyl[1,2,4]triazolo[4,3-a]-1,5-naphthyridine

HRID 42378

反応式

HRID 42378 の反応式
[F:1][CH:2]([F:23])[C:3]1[N:7]2[C:8]3[CH:9]=[C:10]([C:17]4[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=4)[C:11](=O)[NH:12][C:13]=3[CH:14]=[CH:15][C:6]2=[N:5][N:4]=1.O=P(Cl)(Cl)[Cl:26]>C(#N)C>[Cl:26][C:11]1[N:12]=[C:13]2[C:8](=[CH:9][C:10]=1[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[N:7]1[C:3]([CH:2]([F:23])[F:1])=[N:4][N:5]=[C:6]1[CH:15]=[CH:14]2

参加物

4

反応物 2

HCID 24813Phosphorus oxychlorideHCID 670940791-(Difluoromethyl)-8-phenyl-[1,2,4]triazolo[4,3-a][1,5]naphthyridin-7(6H)-one

生成物 1

HCID 582165777-Chloro-1-(difluoromethyl)-8-phenyl[1,2,4]triazolo[4,3-a]-1,5-naphthyridine

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
140 °C

実験手順

A mixture of 1-(difluoromethyl)-8-phenyl[1,2,4]triazolo[4,3-a]-1,5-naphthyridin-7(6H)-one (10-1) (19 g, 61 mmol) and POCl3 (28 mL, 304 mmol) in acetonitrile (95 mL) was heated under microwave irradiation at 140° C. for 2 hours. The solvent was removed under reduced pressure, and to the residue was added water. The resulting solid was collected by filtration to give 7-chloro-1-(difluoromethyl)-8-phenyl[1,2,4]triazolo[4,3-a]-1,5-naphthyridine (10-2) as pale yellow solid.

後処理

  1. customThe solvent was removed under reduced pressure
  2. additionto the residue was added water
  3. filtrationThe resulting solid was collected by filtration

出典と根拠

ORDレコード
ord-6df8a56ef56a427aa34d392e7794f588
出典データセット
uspto-grants-2013_09
特許番号
US08536193B2

関連ノート

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