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Toluene → 8-chlorodibenz[b,f][1,4]oxazepin-10(11H)carbonyl chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Phosgene | HCID 6371 | — |
| 反応物 | 8-Chloro-10,11-dihydrodibenzo[b,f][1,4]oxazepine | HCID 15229227 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | 8-chlorodibenz[b,f][1,4]oxazepin-10(11H)carbonyl chloride | HCID 14975983 | — |
反応手順
13 parts of phosgene in 45 parts of toluene was stirred for 2 hours at 5°-10° C., and then 70 parts of ether was added. This was followed by the addition of a solution of 18.9 parts of 8-chloro-10,11-dihydrodibenz[b,f][1,4]oxazepine and 7.2 parts of triethylamine in 140 parts of ether. After the addition was complete, the mixture was stirred for 2 hours, and then was filtered. The solvent was then evaporated from the filtrate. The resulting residue was then dissolved in 200 parts by volume of hot hexane, and this mixture was then filtered and cooled.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05464830 |
| 出典データセット | uspto-grants-1995_11 |
| ORD ID | ord-6a1780e8a4d341cf88cffeb2aab9ad45 |
| 出典メモ | uspto-grants-1995_11 |