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Phosphorus sulfide (P2S5) → trans-N-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)methanethioamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| 反応物 | trans-N-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)formamide | HCID 86599863 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | trans-N-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)methanethioamide | HCID 86599864 | 81.2% |
反応手順
Phosphorus pentasulfide (5 mg, 0.01 mmol) was added to trans-N-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)formamide (5 mg, 0.015 mmol) in dioxane. The resulting mixture was heated to reflux for 3 h. After evaporation under reduced pressure the crude compound was chromatographed on silica. Elution with toluene/ethyl acetate 85:15 gave trans-N-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)methanethioamide (2.8 mg, 51%). Data: (m/z)=345 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07737136B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-1307a25a8d6f48d0945a334796242a97 |
| 出典メモ | uspto-grants-2010_06 |