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Phosphorus sulfide (P2S5) → 7-Chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| 反応物 | Potassium Sulfide | HCID 162263 | — |
| 反応物 | 7-chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)one | HCID 13726296 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 7-Chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione | HCID 13726301 | 86.1% |
反応手順
To a solution of 20 g (0.07 mole) of 7-chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)-one in 200 ml of toluene was added a mixture of 9.55 g (0.05 mole) of phosphorus pentasulfide and 9.5 g of potassium sulfide which had been ground together. The reaction mixture was filtered and the filtrate concentrated under reduced pressure to give a yellow solid. Recrystallization from absolute ethanol gave 12.5 g (68%) of the product, m.p. 102°-104° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04642343 |
| 出典データセット | uspto-grants-1987_02 |
| ORD ID | ord-6d9483f58f5a4464b36abe0271861de3 |
| 出典メモ | uspto-grants-1987_02 |