Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Phosphorus sulfide (P2S5) → 2-(chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f]-1,4-oxazepine-5(4H)thione
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| 반응물 | 2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepin-5(4H)one hydrochloride | HCID 13726437 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | 2-(chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f]-1,4-oxazepine-5(4H)thione | HCID 13726442 | — |
반응 단계
To a solution of 59 g (0.25 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepin-5(4H)one hydrochloride in 1500 ml of chloroform was added 41.5 g (0.19 mole) of phosphorus pentasulfide and the mixture was heated to reflux for 18 hr. The mixture was filtered and the filtrate was extracted with dilute sodium hydroxide. The chloroform layer was concentrated and the residue was dissolved in 250 ml of boiling isopropyl alcohol. On cooling, 28 g (44%) of yellow solid precipitated. A portion was recrystallized from isopropyl alcohol, m.p. 134°-136° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04727152 |
| 출처 데이터셋 | uspto-grants-1988_02 |
| ORD ID | ord-6e0e6792bd184b57bc64b7b90119b242 |
| 출처 메모 | uspto-grants-1988_02 |