Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Phosphorus sulfide (P2S5) → 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 | 2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)one | HCID 13726293 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 2-(2-Chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione | HCID 13726298 | — |
반응 단계
A mixture of 18.5 g (0.0834 mole) of phosphorus pentasulfide and 18.5 g potassium sulfide was ground together and added to a solution of 100 g (0.417 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)-one in dry toluene, the mixture refluxed 24 hr. and filtered. The filtrate was concentrated and partitioned between chloroform and dilute sodium hydroxide. The chloroform layer was concentrated and the residue was crystallized several times from ethanol. Yield of product was 55 g (52%), m.p. 105°-108° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04642343 |
| 출처 데이터셋 | uspto-grants-1987_02 |
| ORD ID | ord-21d7a9dd016c4ecd87be8b2924ab324c |
| 출처 메모 | uspto-grants-1987_02 |