Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methylamine → 4-(Bromomethyl)-N-methylbenzenesulfonamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methylamine | HCID 6329 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 4-(Bromomethyl)benzenesulfonyl chloride | HCID 2734409 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-(Bromomethyl)-N-methylbenzenesulfonamide | HCID 10015645 | 71% |
반응 단계
Mix 4-(bromomethyl)benzenesulfonyl chloride (2.7 g, 10 mmol), anhydrous potassium carbonate (1.4 g, 10 mmol) and anhydrous THF (60 mL) under nitrogen. Cool the mixture in an ice bath, add dropwise a 2M solution of methylamine in THF, and stir at this temperature for 30 min. Remove the ice bath and stir at ambient temperature for 16 h. Dilute with EtOAc then wash with 1N aqueous HCl. Separate the organic layer, dry over Na2SO4 and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (1:0, 4:1, 7:3 and 13:7) to obtain the title compound (1.5 g, 71%). MS (ES+) m/z: 266 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08580780B2 |
| 출처 데이터셋 | uspto-grants-2013_11 |
| ORD ID | ord-9c3706d5bf73455f8f178b2559803b28 |
| 출처 메모 | uspto-grants-2013_11 |