化工社化工社 化学情報印刷レポート · 研究参考用
Diazepam → 10-chloro-2-chloromethyl-2,3,5,11b-tetrahydro-7-methyl-11b-phenyloxazolo[3,2-d][1,4]benzodiazepin-6(7H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diazepam | HCID 3016 | — |
| 反応物 | Epichlorohydrin | HCID 7835 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 10-chloro-2-chloromethyl-2,3,5,11b-tetrahydro-7-methyl-11b-phenyloxazolo[3,2-d][1,4]benzodiazepin-6(7H)-one | HCID 21409971 | — |
反応手順
A mixture of 10 g. (35 mmole) of 7-chloro-1,3-dihydro-1-methyl-5-phenyl-2H-1,4-benzodiazepin-2-one, 10 g. of aluminum chloride, and 200 ml. of dried benzene was treated with 30 ml. of 1-chloro-2,3-epoxypropane in 100 ml. of benzene. The reaction mixture was stirred overnight. Work-up as in Method A, Example 5, above gave 32 g. of a crude oil. The oil was dissolved in benzene, filtered over Florisil, evaporated to dryness and crystallized from ether-petroleum ether to give the above-titled product as colorless needles, m.p. 140°-142°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04049667 |
| 出典データセット | uspto-grants-1977_09 |
| ORD ID | ord-9e23801453d14c52bc40181f34282f4d |
| 出典メモ | uspto-grants-1977_09 |