Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium Carbonate → 2-Chloro-4-cyano-5-methoxybenzoic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Methyl 2-chloro-4-cyano-5-fluorobenzoate | HCID 67528656 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 2-Chloro-4-cyano-5-methoxybenzoic acid | HCID 67528375 | — |
반응 단계
A mixture of methyl 2-chloro-4-cyano-5-fluorobenzoate (840 mg; 3.93 mmol; 1 eq.) and K2CO3 (2 717.55 mg; 19.66 mmol; 5 eq.) in MeOH (16.80 mL) was stirred at RT for 24 hours. The reaction mixture was concentrated and the residue was taken up in water. The aqueous layer was washed with EtOAc then the aqueous phase was acidified with HCl cc and extracted with EtOAc. The combined organic phases were washed with water, brine, dried over MgSO4 and concentrated affording the title compound as a yellow solid used without further (0.63 g, 75%). 1H NMR (DMSO-d6, 300 MHz) δ 14.05 (br s, 1H), 8.04 (s, 1H), 7.51 (s, 1H), 3.96 (s, 3H). HPLC (Method A) Rt 3.11 min (Purity 88.5%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08202865B2 |
| 출처 데이터셋 | uspto-grants-2012_06 |
| ORD ID | ord-6278cbf234b14c108b446b54b2a79dc3 |
| 출처 메모 | uspto-grants-2012_06 |