Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Bromine → HCID 178517592, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Bromine | HCID 24408 | — |
| 반응물 | 2(1H)-Pyridinone, 3-(trifluoromethyl)- | HCID 3678411 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | HCID 178517592 | HCID 178517592 | 94.2% |
반응 단계
A solution of 2-hydroxy-3-(trifluoromethyl)pyridine (10.0 g) and bromine (3.08 ml, 9.60 g) in methanol (50 ml) was stirred at 20° C. for 22 h. The solution was concentrated and the residue partitioned between ethyl acetate (400 ml) and water (100 ml). The layers were separated and the organic layer was washed with 5% Na2S2O3aq. (100 ml) and brine (100 ml), dried over sodium sulphate, filtered and concentrated. Purified by Biotage SNAP cartridge KP-Sil column twice (100 g, heptane:ethyl acetate=1:0, 3:1 to 2:1) to give 13.69 g light yellow solid as 5-bromo-2-hydroxy-3-(trifluoromethyl)pyridine (95%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09115126B2 |
| 출처 데이터셋 | uspto-grants-2015_08 |
| ORD ID | ord-a9b9b295723d4dd89022c3f180cfbf97 |
| 출처 메모 | uspto-grants-2015_08 |