Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
N-methyl-2-pyrrolidone → 3-Iodo-N-(2-methoxy-1-methyl-ethyl)-5-nitro-benzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 반응물 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | 3-Iodo-5-nitrobenzoic acid | HCID 80580 | — |
| 반응물 | Methoxyisopropylamine | HCID 123458 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3-Iodo-N-(2-methoxy-1-methyl-ethyl)-5-nitro-benzamide | HCID 57851319 | 27.9% |
반응 단계
EDCI (7.07 g, 36.9 mmol) was added in one portion to a stirred solution of 3-Iodo-5-nitro-benzoic acid (2.31 g, 24.6 mmol), HOBt (4.985 g, 36.9 mmol), 2-Amino-1-methoxypropane (2.73 ml, 24.6 mmol) and NMP (4.06 ml 36.9 mmol) in CH2Cl2 (120 ml) and DMF (10 ml) at 0° C. The reaction was allowed to warm to room temperature and was stirred over night. The reaction mixture was then washed with 2N NaOH, water, brine, and dried over Na2SO4. Solvent was removed in vacuo to give 2.50 g of 3-Iodo-N-(2-methoxy-1-methyl-ethyl)-5-nitro-benzamide as a yellow solid, MS (M+H)=365. This material was used without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08846945B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-0d9589c7e058451894f1ce443e0d8999 |
| 출처 메모 | uspto-grants-2014_09 |