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HRID 2046342作成日:2026年10月26日

Triethylamine → Tert-butyl 2-(2-((1-(cyclopropylmethyl)-piperidine-4-yl)(methyl)amino)-2-oxoethoxy)-4,6-dimethylpyrimidine-5-ylcarbamate

https://huagongshe.com/reaction/2046342

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物1-(cyclopropylmethyl)-N-methylpiperidine-4-amineHCID 43314908—
反応物2-(5-(Tert-butoxycarbonylamino)-4,6-dimethylpyrimidine-2-yloxy)acetic acidHCID 59336168—
溶媒AcetonitrileHCID 6342—
生成物Tert-butyl 2-(2-((1-(cyclopropylmethyl)-piperidine-4-yl)(methyl)amino)-2-oxoethoxy)-4,6-dimethylpyrimidine-5-ylcarbamateHCID 5933618152.5%

反応条件

温度25 °C

反応手順

Compound 9 (100 mg), 1-(cyclopropylmethyl)-N-methylpiperidine-4-amine (56.6 mg) and triethylamine (234 μL) were suspended in acetonitrile (2 mL). While the suspension was cooled with ice, a 50% propane phosphonic acid anhydride ethyl acetate solution (273 mg) was added portionwise. The equipment used to add the 50% propane phosphonic acid anhydride ethyl acetate solution was thoroughly washed with acetonitrile (0.5 mL) and was stirred at room temperature (20 to 30° C.) overnight. Subsequently, the reaction mixture was concentrated under reduced pressure and the resulting residue was purified by amino-coated silica gel (Fuji Sylysia Chemical Ltd.; NH-DM1020) column chromatography (methylene chloride:methanol=30:1) to give 79 mg (52% yield) of the desired product as a pale yellow amorphous.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08592435B2
出典データセットuspto-grants-2013_11
ORD IDord-b67e05f06fec4231ac930e33e00f1d99
出典メモuspto-grants-2013_11