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Ethylene Glycol → 7-Chloro-2-(2-hydroxyethoxy)-5-phenyl-3H-1,4-benzodiazepine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylene Glycol | HCID 174 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 7-chloro-2-di-(morpholino)phosphinyloxy-5-phenyl-3H-1,4-benzodiazepin | HCID 14907886 | — |
| 生成物 | 7-Chloro-2-(2-hydroxyethoxy)-5-phenyl-3H-1,4-benzodiazepine | HCID 12284595 | — |
反応手順
A suspension of 1.95 g (4.0 mmoles) of 7-chloro-2-di-(morpholino)phosphinyloxy-5-phenyl-3H-1,4-benzodiazepin in 10 ml of ethylene glycol containing 4 ml of triethylamine was heated on a steam bath for 2 hrs. A clear solution formed soon after heating began. Triethylamine was removed in vacuo. The ethylene glycol solution was poured into ice water precipitating solids which were collected and washed thoroughly with water. Remaining water was removed from the solid by dissolving in solid in ether, drying over sodium sulfate and evaporation of ether. Crystallization of the residue from ether-hexane gave colorless prisms, mp 142°-144°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04739049 |
| 出典データセット | uspto-grants-1988_04 |
| ORD ID | ord-8d84581afc1947669a234219566ec716 |
| 出典メモ | uspto-grants-1988_04 |