Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,2-Dichloroethane → 5-Butyl-pyridine-2-carboxylic acid methoxy-methyl-amide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,2-Dichloroethane | HCID 11 | — |
| 반응물 | Fusaric Acid | HCID 3442 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| 용매 | Sodium Chloride | HCID 5234 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 5-Butyl-pyridine-2-carboxylic acid methoxy-methyl-amide | HCID 58747007 | — |
반응 단계
A mixture of fusaric acid (896 mg, 5.0 mmol), O,N-dimethylhydroxyl-amine hydrochloride (488 mg, 5 mmol), EDC (1.05 g, 5.5 mmol), HOBT (675 mg, 5.0 mmol) and NEt3 (1.4 ml, 10 mmol) in DMF (100 ml) was stirred at room temperature for 2 h. The reaction mixture was diluted with saturated aqueous NaCl and extracted with EtOAc (2×). The combined organic extracts were washed with 0.5 M citric acid, saturated aqueous NaHCO3, saturated aqueous NaCl, dried, and concentrated under vacuum to, give the desired product I-2A-38a as a viscous oil (940 mg): MS 232.2 (M+1)+; 1H NMR (400 MHz, CDCl3) δ 8.40 (s, 1H), 7.60–7.50 (m, 2H), 3.72 (s, 3H), 3.37 (s, 3H), 2.61 (t, 2H, J=7.5Hz), 1.62–1.53 (m, 2H), 1.38–1.28 (m, 2H), 0.89 (t, 3H, J=7.5 Hz).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07141669B2 |
| 출처 데이터셋 | uspto-grants-2006_11 |
| ORD ID | ord-40eb3a178e50452b968a27daaac14ed9 |
| 출처 메모 | uspto-grants-2006_11 |