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HRID 67233作成日:2026年10月25日

Ethanol → 2,3-Bis(o-chlorophenyl)-2,3,5,6,7,8-hexahydrothiazolo[3,2-a][1,3]diazepin-3-ol hydrochloride

https://huagongshe.com/reaction/67233

反応式

関与物質

役割名称HCID仕込み量
反応物EthanolHCID 702—
反応物2-ChlorobenzaldehydeHCID 6996—
反応物Potassium CyanideHCID 9032—
反応物1,3-Diazepane-2-thioneHCID 736589—
溶媒AcetoneHCID 180—
溶媒WaterHCID 962—
生成物2,3-Bis(o-chlorophenyl)-2,3,5,6,7,8-hexahydrothiazolo[3,2-a][1,3]diazepin-3-ol hydrochlorideHCID 20528321—

反応手順

A mixture of 22.6 ml. of o-chlorobenzaldehyde, 8 g. of potassium cyanide and 100 ml. of 65% ethanol is refluxed for 2 hours and then refrigerated. Water (30 ml.) is added, refrigeration is continued, then the water layer is decanted and the oil dissolved in toluene, washed with water, dried and concentrated to an oil. The crude 2,2'-dichlorobenzoin is converted to the methanesulfonate ester as described in Example 1, giving an oil. A 14.6 g. portion of this oil is reacted with 2.6 g. of hexahydro-2H-1,3-diazepin-2-thione in 100 ml. of acetone as described in Example 13, giving 1.4 g. of the desired product, m.p. 224°-226° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04344954
出典データセットuspto-grants-1982_08
ORD IDord-cbe95206ec474485bf42dd91a942cc71
出典メモuspto-grants-1982_08