Potassium Acetate → 2,2,2-Trifluoro-1-(4-hydroxy-5-nitro-10-aza-tricyclo(6.3.1.02,7]dodeca-2(7),3,5-trien-10-yl)-ethanone

関与物質

役割	名称	HCID	仕込み量
反応物	Potassium Acetate	HCID 517044	—
反応物	1-(7,8-Dinitro-1,2,4,5-tetrahydro-3H-1,5-methano-3-benzazepin-3-yl)-2,2,2-trifluoroethan-1-one	HCID 21864744	—
溶媒	Dimethyl Sulfoxide	HCID 679	—
溶媒	Water	HCID 962	—
生成物	2,2,2-Trifluoro-1-(4-hydroxy-5-nitro-10-aza-tricyclo(6.3.1.02,7]dodeca-2(7),3,5-trien-10-yl)-ethanone	HCID 21864728	70%

反応条件

温度	100 °C

反応手順

1-(4,5-Dinitro-10-aza-tricyclo[6.3.1.02,7]dodeca-2(7),3,5-trien-10-yl)-2,2,2-trifluoro-ethanone (900 mg, 2.61 mmol) and potassium acetate (KOAc) (2.6 g, 26.1 mmol) were dissolved in DMSO (10 mL) and warmed with stirring to 100° C. for 16 hours. The mixture was cooled and diluted with H2O (50 mL) then extracted with 80% ethyl acetate/hexanes (6×25 mL). The organic layer was washed with H2O (3×20 mL), dried (Na2SO4), filtered and concentrated and purified by chromatography to give an oil (575 mg, 70%). (TLC 50% ethyl acetate/hexanes (NH3) Rf 0.56)

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US07091372B2
出典データセット	uspto-grants-2006_08
ORD ID	ord-c332f48e15544b4e8f7002466853992f
出典メモ	uspto-grants-2006_08