Cesium carbonate → Alpha-[bis[(1,1-dimethylethoxy)carbonyl]amino]-2-oxo-4-(phenylmethoxy)1(2h)-pyridinepropanoic acid methyl ester

関与物質

役割	名称	HCID	仕込み量
反応物	Cesium carbonate	HCID 10796	—
反応物	4-Benzyloxy-2(1H)-pyridone	HCID 3607724	—
反応物	Methyl 2-(bis((tert-butoxy)carbonyl)amino)prop-2-enoate	HCID 10870342	—
溶媒	Acetonitrile	HCID 6342	—
生成物	Alpha-[bis[(1,1-dimethylethoxy)carbonyl]amino]-2-oxo-4-(phenylmethoxy)1(2h)-pyridinepropanoic acid methyl ester	HCID 58864469	—

反応条件

温度	80 °C

反応手順

To a solution of 2-(di-tert-butoxycarbonylamino)-acrylic acid methyl ester (900 mg, 3.0 mmol), and 4-benzyloxy-1H-pyridin-2-one (630 mg, 1.03 equiv) in acetonitrile (2.5 mL) was added cesium carbonate (100 mg, 0.10 equiv). The resulting suspension was heated to 80° C. via microwave for 2 h. The reaction was concentrated, dissolved in water, and extracted with methylene chloride (3×). The combined organic phases were washed with brine, dried over magnesium sulfate, and concentrated to give 1.47 g (97%) which was used without purification. Mass spec.: 503.56 (MH)+.

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US07220862B2
出典データセット	uspto-grants-2007_05
ORD ID	ord-cf472808937e4b32a2c2e4fe5447d432
出典メモ	uspto-grants-2007_05