3-Chloro-2-butanone → (+/-)-7-(4,5-Dimethyl-thiazol-2-yl)-8-methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine

関与物質

役割	名称	HCID	仕込み量
反応物	3-Chloro-2-butanone	HCID 20026	—
反応物	(+/-)-8-Methyl-5-(4-nitrophenyl)-7-thiocarbamoyl-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine	HCID 12137394	—
溶媒	Dimethylformamide	HCID 6228	—
生成物	(+/-)-7-(4,5-Dimethyl-thiazol-2-yl)-8-methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine	HCID 12137425	76%

反応条件

温度	90 °C

反応手順

A mixture of 0.60 g (1.56 mmol) of the starting material I, 1.02 g (9.57 mmol) of 3-chloro-2-butanone and 8 ml of dimethylformamide was stirred at 90° C. for 3 h. After cooling the precipitated crystals were filtered off, dried and purified by recrystallization from dimethylformamide and water to yield 0.49 g (76%) of the title compound; Mp.: >260° C. (dec.).

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US06858605B2
出典データセット	uspto-grants-2005_02
ORD ID	ord-b8d6d87438154470a19aead526a75785
出典メモ	uspto-grants-2005_02