Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Pyridine → 7-[[(1,1-Dimethylethyl)dimethylsily]oxy]-1,2,3,4-tetrahydro-6-methoxyisoquinoline
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| 반응물 | 7-Methoxy-1,2,3,4-tetrahydroisoquinolin-6-ol | HCID 417289 | — |
| 생성물 | 7-[[(1,1-Dimethylethyl)dimethylsily]oxy]-1,2,3,4-tetrahydro-6-methoxyisoquinoline | HCID 15285554 | — |
반응 단계
To a solution of 19.2 g of 6-hydroxy-7-methoxy-1,2,3,4-tetrahydroisoquinoline in 425 mL of pyridine is added 48.4 g of t-butyl-dimethylsilylchloride and 0.5 g of 4-N,N-dimethylaminopyridine. The solution is heated to reflux for 3.5 hours and the volatiles removed at 70° C. by distillation. The residue is partitioned between aqueous potassium bicarbonate and ethyl acetate. The organic layer is washed with water, dried (magnesium sulfate) and the volatiles removed in vacuo. The residue is suspended in diethyl ether, filtered and washed with hexane. The filtrate is evaporated and the residue distilled via Kugelrohr at 150 mm and 120°-130° C. to afford 26.2 g of the desired product as a colorless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05387685 |
| 출처 데이터셋 | uspto-grants-1995_02 |
| ORD ID | ord-0884c459a87e475f9bd46a231412b209 |
| 출처 메모 | uspto-grants-1995_02 |