Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dichloroacetyl chloride → Benoxacor
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dichloroacetyl chloride | HCID 6593 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 3-Methyl-3,4-dihydro-2H-1,4-benzoxazine | HCID 2763760 | — |
| 용매 | Benzene | HCID 241 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | Benoxacor | HCID 62306 | 83% |
반응 단계
5.3 ml (55 mmoles) of dichloroacetyl chloride are added dropwise, at a temperature of 20° to 25° C. and while stirring, to a suspension of 7.5 g (50 mmoles) of 2,3-dihydro-3-methyl-1,4-benzoxazine and 5.8 g (55 mmoles) of sodium carbonate in 120 ml of benzene. The reaction mixture is then stirred at the same temperature for 30 minutes and is then taken up in a mixture of water and ethyl acetate. The organic phase is washed with saturated sodium chloride solution, dried over sodium sulfate and evaporated. Crystallising the residue from diisopropyl ether gives 10.8 g of 4-dichloroacetyl-2,3-dihydro-3-methyl-1,4-benzoxazine, melting point 105°-107° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04618361 |
| 출처 데이터셋 | uspto-grants-1986_10 |
| ORD ID | ord-e9aaa438dd1e4caf875d550daa2465a4 |
| 출처 메모 | uspto-grants-1986_10 |