Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanol → E-4031 dihydrochloride
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | 2-Ethenyl-6-methylpyridine | HCID 70735 | — |
| 반응물 | Sodium Acetate | HCID 517045 | — |
| 반응물 | N-[4-(piperidine-4-carbonyl)-phenyl]methanesulfonamide hydrochloride | HCID 14130042 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | E-4031 dihydrochloride | HCID 3087190 | 150.7% |
반응 단계
0.254 g (0.797 mmol) of 4-(4-methylsulfonylaminobenzoyl)piperidine hydrochloride, 0.22 g (1.88 mmol) of 6-methyl-2-vinylpyridine and 0.15 g of sodium acetate were suspended in 3 ml of a mixture of methanol and water (1:1) and the suspension was refluxed for 2 h. The liquid reaction mixture was filtered and the filtrate was concentrated. The obtained residue was purified according to silica gel column chromatography (chloroform:methanol:aqueous ammonia=96:4:0.4). The purified product was converted into its hydrochloride with ethanolic hydrogen chloride and recrystallized from ethanol to obtain 0.285 g (yield: 81%) of the intended compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05118689 |
| 출처 데이터셋 | uspto-grants-1992_06 |
| ORD ID | ord-50e352dc85014b8fa31de93c71520f74 |
| 출처 메모 | uspto-grants-1992_06 |