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HRID 1748538作成日:2026年10月25日

Chloroform → HCID 86692490、化合物

https://huagongshe.com/reaction/1748538

反応式

関与物質

役割名称HCID仕込み量
反応物ChloroformHCID 6212—
反応物Potassium Phosphate, TribasicHCID 62657—
反応物Cyclopropylboronic acidHCID 2760897—
反応物Ethyl 1-(5-bromopyridin-2-yl)-5-methylpyrazole-4-carboxylateHCID 46739344—
触媒Dichlorobis(tricyclohexylphosphine)pallium (II)HCID 11050900—
溶媒1,4-DioxaneHCID 31275—
生成物HCID 86692490HCID 8669249088.9%

反応条件

温度110 °C

反応手順

A suspension of 1-(5-bromopyridin-2-yl)-5-methyl-1H-pyrazole-4-carboxylic acid ethyl ester (18 g) described in Reference Example 24 (2), cyclopropylboronic acid (9.96 g), dichlorobis(tricyclohexylphosphine)palladium (II) (2.14 g) and tripotassium phosphate (49.2 g) in 1,4-dioxane (120 ml) was stirred at 110° C. for 3 hours. After completion of the reaction, the mixture was allowed to cool, chloroform was added thereto, filtered through Celite, then, to the filtrate was added a saturated aqueous solution of ammonium chloride, and the mixture was extracted with chloroform. The organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated in vacuo. The obtained residue was purified with silica gel chromatography (n-hexane/ethyl acetate) to give 1-(5-cyclopropylpyridin-2-yl)-5-methyl-1H-pyrazole-4-carboxylic acid ethyl ester (14 g) as a yellow solid. MS (ESI) m/z: 272 (M+H)+.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09150555B2
出典データセットuspto-grants-2015_10
ORD IDord-90b4a38957264d10b70d21734bacc4c0
出典メモuspto-grants-2015_10