Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium Hydroxide → 2-Benzyl-1-bromo-6-methoxypyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | Bromine | HCID 24408 | — |
| 반응물 | Sodium Sulfite | HCID 24437 | — |
| 반응물 | Potassium Bromide | HCID 253877 | — |
| 반응물 | 2-Benzyl-6-methoxypyridine | HCID 21942274 | — |
| 촉매 | Tetraammonium chloride | HCID 22266888 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-Benzyl-1-bromo-6-methoxypyridine | HCID 18182294 | — |
반응 단계
A mixed solution of 17 ml of bromine, 90 g of potassium bromide and 450 ml of water was added dropwise into a mixture of 60 g of 2-benzyl-6-methoxypyridine (Production Example 2-b), 90 g of potassium bromide, 450 ml of water, 20 g of potassium hydroxide and 2.5 g of tetraammonium chloride over 2 hours under stirring in an ice bath. After stirring overnight as it was, sodium sulfite was added thereto and the mixture was extracted with hexane. The organic phase was washed with water and brine, dried over anhydrous magnesium sulfate and the solvent was removed. The residue was subjected to silica gel column chromatography to elute with 0.5-1.5% of ethyl acetate/hexane, to give 72.5 g of the target compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06599917B1 |
| 출처 데이터셋 | uspto-grants-2003_07 |
| ORD ID | ord-0314bc1e8d6b4fe0a3167db30808daec |
| 출처 메모 | uspto-grants-2003_07 |