Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
p-Toluenesulfonic acid → 3-Bromo-4-(dimethoxymethyl)pyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | p-Toluenesulfonic acid | HCID 6101 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | 3-Bromopyridine-4-carboxaldehyde | HCID 2762997 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Hexane | HCID 8058 | — |
| 생성물 | 3-Bromo-4-(dimethoxymethyl)pyridine | HCID 20715145 | 93.5% |
반응 단계
PTSA (834 mg, 4.384 mmol) was added to a solution of 3-bromo-pyridine-4-carbaldehyde (600 mg, 3.2256 mmol) in methanol (20 mL). The resulting mixture was heated to reflux for 4 hours. The reaction was monitored by TLC (20% ethylacetate in hexane). The reaction mixture was concentrated and basified with NaHCO3 solution. The reaction mixture was partitioned between water and DCM. The organic layer was washed with brine solution, dried over Na7SO4, filtered and the filtrate was concentrated to afford 700 mg of 3-Bromo-4-dimethoxymethyl-pyridine (93.5% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | USRE045173E1 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-01d6cc1ef2a0457f8f9467b2d8223657 |
| 출처 메모 | uspto-grants-2014_09 |