Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
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
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| 반응물 | 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 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 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% |
반응 단계
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)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07737136B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-1307a25a8d6f48d0945a334796242a97 |
| 출처 메모 | uspto-grants-2010_06 |