Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → N-(2-Methyl-2-propenyl)-3-[4-(trifluoromethyl)phenoxy]-1-azetidinecarboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 반응물 | 2-Methylallylamine | HCID 76141 | — |
| 반응물 | 3-[4-(Trifluoromethyl)phenoxy]azetidine oxalate | HCID 12812500 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | N-(2-Methyl-2-propenyl)-3-[4-(trifluoromethyl)phenoxy]-1-azetidinecarboxamide | HCID 15053426 | 58.9% |
반응 단계
A stirred solution of 3.6 g (0.022 mole) of 1,1'-carbonyldiimidazole in 75 ml of methylene chloride under nitrogen was treated with 1.6 g (0.022 mole) of 2-methyl-2-propenylamine (added via a syringe and needle through a septum placed in one neck of the reaction flask). After stirring for 1 hr, 6.2 g (0.02 mole) of 3-[4-(trifluoromethyl)phenoxy]azetidine oxalate was added all at once followed in 30 min with 5 ml of triethylamine and stirring was continued for 3 hr. The reaction mixture was washed with water (2×25 ml), dried over magnesium sulfate and concentrated in vacuo. The oily residue solidified on standing and was recrystallized from isopropyl ether to yield 3.7 g (58.9%) of fine white crystals, m.p. 101°-102° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05068231 |
| 출처 데이터셋 | uspto-grants-1991_11 |
| ORD ID | ord-2c6dd84aad9f4a2e9b20996cd93451c3 |
| 출처 메모 | uspto-grants-1991_11 |