Phosphorus oxychloride → 1-Chloro-3-(2,4,5-trimethoxyphenyl)isoquinoline

HRID 1006874

反応式

HRID 1006874 の反応式
[CH3:1][NH:2][C:3]([C:5]1[C:6]([CH3:11])=[CH:7][CH:8]=[CH:9][CH:10]=1)=O.[CH3:12][O:13][C:14]1[CH:21]=[C:20]([O:22][CH3:23])[C:19]([O:24][CH3:25])=[CH:18][C:15]=1C#N.P(Cl)(Cl)([Cl:28])=O>>[Cl:28][C:3]1[C:5]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:11]=[C:1]([C:15]2[CH:18]=[C:19]([O:24][CH3:25])[C:20]([O:22][CH3:23])=[CH:21][C:14]=2[O:13][CH3:12])[N:2]=1

参加物

4

実験手順

3-(2,4,5-Trimethoxyphenyl)isoquinolin-1-one obtained by reacting N-methyl-o-toluamide (1.50 g) and 2,4,5-trimethoxybenzonitrile (1.93 g) according to Example 10-1 was reacted with phosphorous oxychloride (10 ml) according to Example 10-2, to give 1-chloro-3-(2,4,5-trimethoxyphenyl)isoquinoline, which was then reacted with N-ethylpiperazine (15 ml) at 120° C. for 5 hr. The reaction solution was evaporated, and to the resulting residue were added ethyl acetate and water. The resulting organic layer was wahsed with water and brine, and then dried over magnesium sulfate. The solvent was evaporated, and the reuslting residue was purified by silica gel column chromatography (methylene chloride/methanol system), to give the free compound of the title compound as a pale yellow oil.

出典と根拠

ORDレコード
ord-5003193267274f079e7799fa85c1f077
出典データセット
uspto-grants-2004_09
特許番号
US06790844B2

関連ノート

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