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HRID 357486作成日:2026年10月25日

Potassium Carbonate → HCID 15611948、化合物

https://huagongshe.com/reaction/357486

反応式

関与物質

役割名称HCID仕込み量
反応物Potassium CarbonateHCID 11430—
反応物Benzoic acid, 2-hydroxy-3-methyl-, methyl esterHCID 31835—
反応物Sodium methanesulfinateHCID 2733271—
反応物2-Chloro-4,6-dimethoxypyrimidineHCID 5152323—
溶媒DimethylformamideHCID 6228—
生成物HCID 15611948HCID 15611948—

反応手順

4.38 g (25 mmol) of 2-chloro-4,6-dimethoxypyrimidine, 4.17 g (25.0 mmol) of methyl 2-hydroxy-3-methylbenzoate and 0.66 g (6.3 mmol) of sodium methanesulfinate were heated in the presence of 5.17 g (37.5 mmol) of potassium carbonate in 25 ml of N,N-dimethylformamide to 120° C. with stirring. After 8 hours, the solvent was removed in a rotary evaporator at 60° C./20 mbar. The residue was taken up in 30 ml of water and 30 ml of dichloromethane. After the organic phase had been separated off, the aqueous phase was again extracted with 20 ml of dichloromethane. The combined organic phases was washed with water, dried over magnesium sulfate and evaporated. The residue was purified by chromatography on a silica gel column (eluent hexane/ethyl acetate 4:1). The title product was obtained from the product fraction in a yield of 5.23 g (65.8 percent of theory) (GC content 96 percent). The melting point of the compound was 73.8° to 79.1° C. Other data concerning the title compound was:

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05840892
出典データセットuspto-grants-1998_11
ORD IDord-aefd827c51644e598e3a91380a52eda0
出典メモuspto-grants-1998_11