Methanol → 3-Methoxysulfonylamino-3-methyl-N-[2,3,4,5-tetrahydro-2-oxo-1H-1-benzazepin-3(R)-yl]butanamide

関与物質

役割	名称	HCID	仕込み量
反応物	Methanol	HCID 887	—
反応物	Triethylamine	HCID 8471	—
反応物	(R)-3-amino-4,5-dihydro-1H-benzo[b]azepin-2(3H)-one	HCID 10103689	—
反応物	2,2-Dimethyl-4-oxoazetidine-1-sulfonyl chloride	HCID 10943445	—
生成物	3-Methoxysulfonylamino-3-methyl-N-[2,3,4,5-tetrahydro-2-oxo-1H-1-benzazepin-3(R)-yl]butanamide	HCID 10861558	—

反応条件

温度	0 °C

反応手順

A suspension of 98.31 g (0.530 mol) of 3(R)-amino-2,3,4,5-tetrahydro-1H-1-benzazepin-2-one in 1600 mL of methanol at room temperature was treated with 155 mL (1.112 mol) of triethylamine. The resulting suspension was cooled to 0° C. and treated with a solution of 110.01 g (0.557 mol) of N-chlorosulfonyl-4,4-dimethylazetidin-2-one in 960 mL of methanol over 20 minutes maintaining the internal temperature below 10° C. Additional methanol (100 mL) was used to rinse the flask and the rinse was transferred into the reaction vessel. The reaction mixture was warmed to room temperature and stirred for 90 minutes.

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US05206235
出典データセット	uspto-grants-1993_04
ORD ID	ord-af771d7d163946a1aaf62632898509db
出典メモ	uspto-grants-1993_04