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HRID 42191作成日:2026年10月25日

Hydrochloric Acid → HCID 59240648、化合物

https://huagongshe.com/reaction/42191

反応式

関与物質

役割名称HCID仕込み量
反応物Hydrochloric AcidHCID 313—
反応物TriethylamineHCID 8471—
反応物1-Benzyl-4-chlorophthalazineHCID 6404566—
反応物(S)-4-(5-Methoxycarbonyl-4-trifluoromethyl-pyrimidin-2-yl)-piperazine-1,3-dicarboxylic acid 1-tert-butyl ester 3-methyl-esterHCID 68707290—
溶媒Diethyl EtherHCID 3283—
溶媒DichloromethaneHCID 6344—
生成物HCID 59240648HCID 592406488%

反応手順

To a methylene chloride (0.02M) solution of (S)-4-(5-Methoxycarbonyl-4-trifluoromethyl-pyrimidin-2-yl)-piperazine-1,3-dicarboxylic acid 1-tert-butyl ester 3-methyl-ester (69 mg, 0.153 mmol), is added 1N HCl (2 mmol), 2M in diethyl ether. Stir reaction mixture at room temperature for 18 h. Concentrate and dilute with dioxane (0.1 M), followed by addition of 1-benzyl-4-chloro-phthalazine (0.153 mmol) and triethylamine (0.459 mmol). Microwave reaction mixture for 30 min at 150° C. MS shows some starting material still present. Microwave for an additional 2.5 h at 150° C. Concentrate reaction mixture and purify by column chromatography 0-75% ethyl acetate/heptane gradient to afford the title compound. (8% yield)

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08536168B2
出典データセットuspto-grants-2013_09
ORD IDord-1fb9fdad713d49a7b704ceef49f7cac2
出典メモuspto-grants-2013_09