Acetic Acid → (+)-9-{6-[(4-Methoxy-benzyl)-methyl-amino]-pyridin-2-yl}-3-pyrimidin-5-yl-non-4-enoic acid ethyl ester

関与物質

役割	名称	HCID	仕込み量
反応物	Acetic Acid	HCID 176	—
反応物	Formaldehyde	HCID 712	—
反応物	Sodium cyanoborohydride	HCID 5003444	—
反応物	(+)9-[6-(4-Methoxy-benzylamino)-pyridin-2-yl]-3-pyrimidin-5-yl-non-4-enoic acid ethyl ester	HCID 69666458	—
溶媒	Methanol	HCID 887	—
生成物	(+)-9-{6-[(4-Methoxy-benzyl)-methyl-amino]-pyridin-2-yl}-3-pyrimidin-5-yl-non-4-enoic acid ethyl ester	HCID 69665963	75%

反応条件

温度	50 °C

反応手順

To a solution of 6-10 (1.6 g, 3.37 mmol) in methanol (30 mL) was added paraformaldehyde (0.80 g) and acetic acid (0.96 mL, 16.8 mmol). After stirring at 50° C. for 15 minutes, NaCNBH3 (0.275 g, 4.38 mmol) was added and the mixture stirred for an additional 30 minutes at 50° C. Evaporation of the solvents and purification on silica gel (5% MeOH/CHCl3) afforded 6-10 in 75% yield.

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US07153862B2
出典データセット	uspto-grants-2006_12
ORD ID	ord-d79e5cceb1c549358ec1f02e0e0b5fc7
出典メモ	uspto-grants-2006_12