Potassium Carbonate → 1,1-Dimethylethyl 4-[(3'-cyano-3-biphenylyl)methylidene]-1-piperidinecarboxylate

関与物質

役割	名称	HCID	仕込み量
反応物	Potassium Carbonate	HCID 11430	—
反応物	1,4-Dioxane	HCID 31275	—
反応物	Tert-butyl 4-(3-bromobenzylidene)piperidine-1-carboxylate	HCID 57813409	—
触媒	HCID 178418397	HCID 178418397	—
溶媒	Water	HCID 962	—
生成物	1,1-Dimethylethyl 4-[(3'-cyano-3-biphenylyl)methylidene]-1-piperidinecarboxylate	HCID 67005869	86%

反応条件

温度	130 °C

反応手順

To 1,1-dimethylethyl 4-[(3-bromophenyl)methylidene]-1-piperidinecarboxylate (2.11 g, 5.99 mmol) in 1,4-dioxane (30 mL) and water (10.00 mL) was added m-NC(C6H4)B(OH)2 (1.056 g, 7.19 mmol), Pd(Ph3P)4 0.277 g, 0.240 mmol), and K2CO3 (2.483 g, 17.97 mmol). The resultant mixture was split into two equal portions and each portion was heated in a microwave at 130° C. for 15 min. The reaction mixture was concentrated by Glas-Col evaporator and purified with CombiFlash chromatograph to afford the title compound (1.93 g, 86%). LC-MS m/z 749 (2M+H)+.

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US08067408B2
出典データセット	uspto-grants-2011_11
ORD ID	ord-30601844cad54c518aefb18ae3cfb373
出典メモ	uspto-grants-2011_11