Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Carbon Dioxide → 2,6-Dichloro-4-methoxynicotinic Acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Carbon Dioxide | HCID 280 | — |
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 2,6-Dichloro-4-methoxypyridine | HCID 3319993 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2,6-Dichloro-4-methoxynicotinic Acid | HCID 59310097 | 70% |
반응 단계
To a solution of 4.0 g (22.5 mmol) 2,6-dichloro-4-methoxy-pyridine in THF (20 ml) was added 10.0 ml (2.47 M in hexane, 24.7 mmol) n-butyllithium at −78° C. After stirring for 1 h at −78° C. excess dry ice was added and the mixture was allowed to warm to RT. Then the mixture was acidified with 6N aqueous hydrochlorid acid to pH 3-4 followed by extraction with EtOAc. The organic layer was dried over Na2SO4 and concentrated in vacuo. Purification of the residue by CC (hexane/EtOAc 4:1) provided 3.5 g (15.8 mmol, 70%) 2,6-dichloro-4-methoxy-pyridine-3-carboxylic acid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09168259B2 |
| 출처 데이터셋 | uspto-grants-2015_10 |
| ORD ID | ord-b5cb3af8d0bc471aa893c4a3d9339619 |
| 출처 메모 | uspto-grants-2015_10 |