Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Phosphorus sulfide (P2S5) → 7-Chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| 반응물 | Potassium Sulfide | HCID 162263 | — |
| 반응물 | 7-chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)one | HCID 13726296 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 7-Chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione | HCID 13726301 | 86.1% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04727152 |
| 출처 데이터셋 | uspto-grants-1988_02 |
| ORD ID | ord-8c189722a6464305b05c5f2ecbd00eea |
| 출처 메모 | uspto-grants-1988_02 |