Phosphorus oxychloride → 1-Chloro-3-(4-trifluoromethoxyphenyl)isoquinoline

HRID 1251206

反応式

HRID 1251206 の反応式
[F:1][C:2]([F:22])([F:21])[O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[NH:11][C:12](=O)[C:13]3[C:18]([CH:19]=2)=[CH:17][CH:16]=[CH:15][CH:14]=3)=[CH:6][CH:5]=1.P(Cl)(Cl)([Cl:25])=O>>[Cl:25][C:12]1[C:13]2[C:18](=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:19]=[C:10]([C:7]2[CH:8]=[CH:9][C:4]([O:3][C:2]([F:22])([F:21])[F:1])=[CH:5][CH:6]=2)[N:11]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 225032223-(4-Trifluoromethoxyphenyl)isoquinolin-1-one

生成物 1

HCID 225028651-Chloro-3-(4-trifluoromethoxyphenyl)isoquinoline

実験手順

The resulting 3-(4-trifluoromethoxyphenyl)isoquinolin-1-one (3.01 g) was reacted with phosphorus oxychloride (20 ml) according to the method of Example 10-2, to give 1-chloro-3-(4-trifluoromethoxyphenyl)isoquinoline, which was then reacted as it was with N-ethylpiperazine (40 ml) at 90° C. overnight. The reaction solution was evaporated, and to the resulting residue were added ethyl acetate and purified water. The ethyl acetate layer was washed with water and brine, and dried over magnesium sulfate. The solvent was evaporated, and the resulting residue was purified by silica gel column chromatography (chloroform/methanol system), to give 3.65 g of the free compound of the title compound as a pale yellow oil.

出典と根拠

ORDレコード
ord-85eb97423aba4a1da1e34c8c940b5f41
出典データセット
uspto-grants-2002_01
特許番号
US06340759B1

関連ノート

読み込み中…