Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
N-Methylpropylamine → Methyl 3-iodo-5-{[methyl(propyl)amino]carbonyl}benzoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | N-Methylpropylamine | HCID 12315 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 반응물 | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| 반응물 | 3-Iodo-5-(methoxycarbonyl)benzoic acid | HCID 15840391 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Methyl 3-iodo-5-{[methyl(propyl)amino]carbonyl}benzoate | HCID 21086185 | 75.3% |
반응 단계
Mix 5-iodo-isophthalic acid monomethyl ester (3.6 g), N-methyl propyl amine (1.2 mL, 11.8 mmol), 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (2.3 g, 11.8 mmol), and 1-hydroxybenzotriazole hydrate (1.6 g, 11.8 mmol) in dichloromethane (40 mL) and stir at room temperature for 4 h. Dilute with dichloromethane (20 mL), wash with water, 5% aqueous ammonium chloride solution, 5% aqueous sodium bicarbonate solution. Dry (sodium sulfate), concentrate and purify (silica gel chromatography, eluting with ethyl acetate and hexanes) to give the title compound (3.2 g, 74%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07585885B2 |
| 출처 데이터셋 | uspto-grants-2009_09 |
| ORD ID | ord-2ae68db5ccde4037ab94d90d82891dce |
| 출처 메모 | uspto-grants-2009_09 |