Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Tetrahydrofuran → 5,6-dichloro-N-[3-(dimethylamino)propyl]-N-methylpyridine-3-sulfonamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 1,3-Propanediamine, N1,N1,N3-trimethyl- | HCID 78302 | — |
| 반응물 | 5,6-dichloropyridine-3-sulfonyl Chloride | HCID 4736911 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 5,6-dichloro-N-[3-(dimethylamino)propyl]-N-methylpyridine-3-sulfonamide | HCID 64608804 | 69% |
반응 단계
With cooling with ice, triethylamine (0.57 ml, 4.06 mmol) and N,N,N′-trimethylpropane-1,3-diamine (0.34 ml, 2.23 mmol) were added to a tetrahydrofuran solution (5 ml) of 5,6-dichloropyridin-3-sulfonyl chloride (500 mg, 2.03 mmol), and stirred for 5 minutes. Saturated saline water was added to the reaction solution, extracted with chloroform, and the organic layer was dried over anhydrous sodium sulfate, concentrated under reduced pressure. The obtained residue was purified by amine-type silica gel column chromatography (Biotage NH, hexane:ethyl acetate=6:1 to 4:1) to obtain 5,6-dichloro-N-[3-(dimethylamino)propyl]-N-methylpyridine-3-sulfonamide (454 mg, yield: 69%) as a red solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08232284B2 |
| 출처 데이터셋 | uspto-grants-2012_07 |
| ORD ID | ord-f911b62979b0430e850da44cfa5ab343 |
| 출처 메모 | uspto-grants-2012_07 |