Potassium Carbonate → 4-[6-(5-Methanesulfonyl-2,3-dihydro-indol-1-yl)-pyrimidin-4-ylamino]-piperidine-1-carboxylic acid tert-butyl ester

関与物質

役割	名称	HCID	仕込み量
反応物	Potassium Carbonate	HCID 11430	—
反応物	Dimethylacetamide	HCID 31374	—
反応物	4-Amino-1-Boc-piperidine	HCID 1268291	—
反応物	1-(6-Chloropyrimidin-4-yl)-5-(methylsulfonyl)indoline	HCID 59566526	—
溶媒	Sodium chloride; water	HCID 57417360	—
生成物	4-[6-(5-Methanesulfonyl-2,3-dihydro-indol-1-yl)-pyrimidin-4-ylamino]-piperidine-1-carboxylic acid tert-butyl ester	HCID 58074125	—

反応条件

温度	80 °C

反応手順

A mixture of 6a (0.4 g, 1.29 mmol), 4-amino-piperidine-1-carboxylic acid tert-butyl ester (0.4 g, 1.5 eq), DMA (5 mL) and potassium carbonate (0.4 g, 2.2 eq) was heated at 80° C. for 42 h. After allowing the reaction mixture to cool down to room temperature, 100 mL of brine was added and the mixture was extracted with ethyl acetate twice (100 mL and 30 mL). The combined extracts were washed with brine (2×50 mL), dried over magnesium sulfate and filtered. The solvent was removed under vacuum to give a solution of 6b in DMA.

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US08481731B2
出典データセット	uspto-grants-2013_07
ORD ID	ord-4a1b421ad8224d65bd9a3b41614f8ef6
出典メモ	uspto-grants-2013_07