関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Amino-2-propanol | HCID 4 | — |
| 反応物 | O-Xylene | HCID 7237 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | N-(2-benzoyl-4-chlorophenyl)-2-bromoacetamide | HCID 122906 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Oxazolam | HCID 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
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US03997591 |
|---|
| 出典データセット | uspto-grants-1976_12 |
|---|
| ORD ID | ord-31eca73ceb2b45fe853685b5edca807f |
|---|
| 出典メモ | uspto-grants-1976_12 |
|---|