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HRID 492130作成日:2026年10月27日

Toluene → 5-Chloro-3-(4,6-dimethoxypyrimidine-2-yl)-2-methylindole

https://huagongshe.com/reaction/492130

反応式

関与物質

役割名称HCID仕込み量
反応物TolueneHCID 1140—
反応物Ethyl AcetateHCID 8857—
反応物Hydrazine, (4-chlorophenyl)-, hydrochloride (1:1)HCID 71600—
反応物1-(4,6-Dimethoxypyrimidin-2-yl)propan-2-oneHCID 11264052—
触媒ZincchlorideHCID 3007855—
溶媒WaterHCID 962—
生成物5-Chloro-3-(4,6-dimethoxypyrimidine-2-yl)-2-methylindoleHCID 1785676684%

反応手順

To 80 ml of toluene were added 8.0 g (40 m moles) of 1-(4,6-dimethoxypyrimidine-2-yl)-2-propanone and 7.9 g (44 m moles) of 4-chlorophenylhydrazine hydrochloride. Thereto was added 6.54 g (48 m moles) of zinc chloride. Refluxing was made for 2 hours with heating. The reaction mixture was allowed to cool. Then, ethyl acetate and water were added to dissolve the whole reaction mixture. The organic layer was washed with water, separated, and dried over Glauber's salt. The resulting organic layer was concentrated under reduced pressure using a rotary evaporator to obtain an orange solid. The solid was washed with isopropyl ether to obtain 10.2 g (33.7 m moles) of 5-chloro-3-(4,6-dimethoxypyrimidine-2-yl)-2-methylindole. Yield: 84% Melting point: 179 to 181° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07531654B2
出典データセットuspto-grants-2009_05
ORD IDord-ead58d8be5a34a75b626e3cf4bce05b5
出典メモuspto-grants-2009_05