Potassium Phosphate, Tribasic → Isobutyl 1-(3-(2-hydroxyphenyl)isoquinolin-1-yl)piperidin-4-ylcarbamate

関与物質

役割	名称	HCID	仕込み量
反応物	Potassium Phosphate, Tribasic	HCID 62657	—
反応物	1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)	HCID 636044	—
反応物	2-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)phenol	HCID 2734622	—
反応物	HCID 86612202	HCID 86612202	—
触媒	palladium(II) acetate	HCID 167845	—
溶媒	Water	HCID 962	—
溶媒	Toluene	HCID 1140	—
生成物	Isobutyl 1-(3-(2-hydroxyphenyl)isoquinolin-1-yl)piperidin-4-ylcarbamate	HCID 135501906	—

反応条件

温度	150 °C

反応手順

A mixture of 1-(3-chloroisoquinolin-1-yl)piperidin-4-ylcarbamate (99 mg, 0.27 mmol), 2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-phenol (92 mg, 0.42 mmol), K3PO4 (0.17 g, 0.80 mmol), Pd(OAc)2 (3.9 mg, 17 μmol), Xantphos (6.6 mg, 11 μmol), toluene (1.3 mL), and water (0.1 mL) was sealed in a microwave vessel and heated by microwave irradiation at 150° C. for 10 minutes. The reaction was filtered and purified by reverse phase HPLC (10%-99% CH3CN (0.035% TFA)/H2O (0.05% TFA)) to yield isobutyl 1-(3-(2-hydroxyphenyl)isoquinolin-1-yl)piperidin-4-ylcarbamate. LC/MS: m/z 420.2 (M+H)+ at 3.79 min (10%-99% CH3CN (0.035% TFA)/H2O (0.05% TFA)).

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US08372843B2
出典データセット	uspto-grants-2013_02
ORD ID	ord-cddce82c4ce649b0bc18fb1f3c0266e0
出典メモ	uspto-grants-2013_02