Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methylamine → 3-iodo-N-methylbenzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methylamine | HCID 6329 | — |
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | 3-Iodobenzoyl chloride | HCID 74378 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3-iodo-N-methylbenzamide | HCID 3384366 | 26% |
반응 단계
To a cooled (0° C.) solution of 3-iodobenzoyl chloride (2.66 g; 10.0 mmol) in DCM (10 mL) was slowly added a 2 M solution of methylamine in THF (10 mL, 2.0 eq.). Upon completion of the addition, the ice bath was removed and the mixture was stirred overnight. All volatiles were removed in vacuo and the residue was treated with aq. NaHCO3 (25 mL) and subsequently extracted with ethyl acetate (3×15 mL). The combined organic layers were dried over MgSO4 and evaporated. The crude product was purified by column chromatography on silica gel to give the desired 3-iodo-N-methylbenzamide (0.67 g, 26% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08524724B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-2ccd5342a78a44c68040cb5a8f689b09 |
| 출처 메모 | uspto-grants-2013_09 |