Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Phosgene → 1-Chlorocarbonyl-3-[3-(trifluoromethyl)phenoxy]azetidine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Phosgene | HCID 6371 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 1-Benzhydryl-3-[3-(trifluoromethyl)phenoxy]azetidine | HCID 11728694 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1-Chlorocarbonyl-3-[3-(trifluoromethyl)phenoxy]azetidine | HCID 19799606 | 62% |
반응 단계
A solution of 35.6 g (0.36 mole) of phosgene in 200 ml of methylene chloride at 5° C. was stirred with 50 g (0.36 mole) of potassium carbonate for 1 hr. To the mixture was added dropwise 115 g (0.3 mole) of 1-diphenylmethyl-3-[-3-(trifluoromethyl)phenoxy]azetidine in 400 ml of methylene chloride. After stirring for 18 hr, the reaction mixture was filtered and the filtrate was washed with water, dried over magnesium sulfate and concentrated on a rotary evaporator to a viscous oil residue, 133.2 g. Trituration of the residue with hexane gave a solid which was recrystallized from cold hexane to yield 52 g (62%) of white crystals, m.p. 72.5°-74° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05068231 |
| 출처 데이터셋 | uspto-grants-1991_11 |
| ORD ID | ord-af588826d4cf4c0aaa532385c2c04d5a |
| 출처 메모 | uspto-grants-1991_11 |