Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 2-Methyl-6-(trifluoromethyl)nicotinic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 반응물 | Methyl 2-methyl-6-(trifluoromethyl)nicotinate | HCID 2779428 | — |
| 용매 | Methanol--water (1/1) | HCID 22242641 | — |
| 생성물 | 2-Methyl-6-(trifluoromethyl)nicotinic acid | HCID 2775683 | 90.9% |
반응 단계
6.68 g (0.0305 mol) of 2-methyl-6-trifluoromethyl-nicotinic acid methyl ester (prepared in the manner described in Heterocycles, 46, 129 (1997)) are dissolved in 250 ml of methanol/water (3:1 mixture) and 1.92 g (0.046 mol) of lithium hydroxide hydrate are added in portions at 22° C. After 4 hours at 22° C., the reaction mixture is added to ethyl acetate and 2N hydrochloric acid; the organic phase is washed three times with water, dried with sodium sulfate and concentrated by evaporation, and the residue is triturated with a small amount of hexane. After filtering, 5.69 g (90% of theory) of the expected 2-methyl-6-trifluoromethyl-nicotinic acid having a melting point of 147-149° C. are obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06890885B2 |
| 출처 데이터셋 | uspto-grants-2005_05 |
| ORD ID | ord-6786c08f58184e3793d5a6323c3caed0 |
| 출처 메모 | uspto-grants-2005_05 |