Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → Ethyl 2-(4,5-dichloro-2-hydroxyphenylamino)acetate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Ethyl oxoacetate | HCID 70211 | — |
| 반응물 | 2-Amino-4,5-dichlorophenol | HCID 3015415 | — |
| 반응물 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Ethyl 2-(4,5-dichloro-2-hydroxyphenylamino)acetate | HCID 117610965 | 81% |
반응 단계
To a solution of 2-amino-4,5-dichlorophenol (2.0 g, 11.3 mmol) and ethyl-2-oxoacetate (2.26 g, 12.42 mmol) in DCM (50 mL) at room temperature, AcOH (1 mL) was added and the resulting mixture was stirred for 1 h. To this mixture, NaBH(OAc)3 (7.2 g, 33.9 mmol) was added and then stirred for 16 h. The mixture was concentrated in vacuo and the residue was suspended in DCM. The mixture was filtered through a pad of Celite and the filtrate was washed with brine. The organic layer was dried over anhydrous Na2SO4, filtered and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel (petroleum ether/ethyl acetate=10:1) to afford the desired product (2.4 g, 81% yield) as a solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09227978B2 |
| 출처 데이터셋 | uspto-grants-2016_01 |
| ORD ID | ord-0b276b5a9d03459dbf4f44630f146cfb |
| 출처 메모 | uspto-grants-2016_01 |