Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methylamine → 4-iodo-N-methyl-3-nitrobenzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methylamine | HCID 6329 | — |
| 반응물 | Thionyl Chloride | HCID 24386 | — |
| 반응물 | 4-Iodo-3-nitrobenzoic acid | HCID 11208598 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 4-iodo-N-methyl-3-nitrobenzamide | HCID 20755545 | 62.3% |
반응 단계
10 g (0.034 mol) 4-Iodo-3-nitrobenzoic acid (Compound VI-1) and 50 ml N,N-dimethylformamide were added into a reaction flask, stirred to dissolve, and cooled to below 10° C., and 7.5 ml (0.10 mol) sulfoxide chloride was added. After completion of the dropwise addition, the mixture was warmed to room temperature and reacted for one hour. The reaction mixture was poured into 200 ml aqueous solution of 30% methylamine with low temperature, stirred for 5 minutes to precipitate a solid, and then the mixture was added with 500 ml ice-water, stirred for 10 minutes, filtered. The solid was washed with water and dried to obtain N-methyl-4-iodo-3-nitrobenzamide (Compound VII-1), 6.5 g (0.021 mol), yield 62.3%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08946478B2 |
| 출처 데이터셋 | uspto-grants-2015_02 |
| ORD ID | ord-81194174e91445f69f6c4315a4903ca9 |
| 출처 메모 | uspto-grants-2015_02 |