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HRID 328492作成日:2026年10月27日

1-Amino-2-propanol → Oxazolam

https://huagongshe.com/reaction/328492

反応式

関与物質

役割名称HCID仕込み量
反応物1-Amino-2-propanolHCID 4—
反応物O-XyleneHCID 7237—
反応物TriethylamineHCID 8471—
反応物N-(2-benzoyl-4-chlorophenyl)-2-bromoacetamideHCID 122906—
溶媒ChloroformHCID 6212—
溶媒HexaneHCID 8058—
溶媒Ethyl AcetateHCID 8857—
生成物OxazolamHCID 4617—

反応手順

A solution of 67 g. (0.19 mole) of 2-(2-bromoacetamido)-5-chloro-benzophenone, 500 ml. of xylene, 15.7 g. (0.21 mole) of 1-amino-2-propanol and 25 ml. of triethylamine was stirred at reflux for 20 hours. The reaction mixture was concentrated in vacuo to a residue which was partitioned between methylene chloride and water. The organic layer was washed with water, dried and concentrated to an oil which was crystallized from ethyl acetate to give 18.3 g. of a colorless solid, m.p. 181°-184°. Thin layer chromatography on Eastman alumina plates with an eluant of 3 parts of hexane and 2 parts of ethyl acetate revealed the presence of two compounds. The product was dissolved in chloroform and chromatographed over Woelm neutral alumina I. A mixture concentrated in the above-titled product (the faster of the two compounds) was collected in 30% ethyl acetate-70% hexane. Recrystallizations from methylene chloride gave colorless prisms, m.p. 188°-189°.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04017532
出典データセットuspto-grants-1977_04
ORD IDord-d5741bd353a44323a7015ea180e5d856
出典メモuspto-grants-1977_04