Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
p-Toluenesulfonic acid monohydrate → [(R)-1-(5-Bromo-3-methyl-pyridin-2-yl)-pyrrolidin-3-yl]-dimethyl-amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 반응물 | 2,5-Dibromo-3-methylpyridine | HCID 817680 | — |
| 반응물 | (3R)-(+)-3-(Dimethylamino)pyrrolidine | HCID 2758521 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | [(R)-1-(5-Bromo-3-methyl-pyridin-2-yl)-pyrrolidin-3-yl]-dimethyl-amine | HCID 66673852 | 99% |
반응 단계
Combine 2,5-dibromo-3-methyl-pyridine (2.00 g, 7.97 mmol) with dimethyl-(R)-pyrrolidin-3-yl-amine (2.40 g, 20.72 mmol) and p-toluenesulfonic acid monohydrate (0.39 g, 2.07 mmol) in a sealed tube and heat at 100° C. overnight. Dilute with EtOAc (100 mL), wash with saturated NaHCO3 (3×40 mL), dry over Na2SO4, filter and concentrate. Purify the crude material by chromatography, eluting with 2% NH3H2O in 1:1 CH3OH:EtOAc to give 2.09 g (99%) of the title compound. LC-MS/ES m/z (79Br) 284.3 [M+H]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08101764B2 |
| 출처 데이터셋 | uspto-grants-2012_01 |
| ORD ID | ord-47b41fdcf37f467cb71fdf6c783827d3 |
| 출처 메모 | uspto-grants-2012_01 |