Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → Tolterodine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | N,N-diisopropyl-3-phenyl-3-(2-hydroxy-5-methylphenyl)propionamide | HCID 11551832 | — |
| 반응물 | Aluminium lithium hydride | HCID 21226445 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | Tolterodine | HCID 443879 | 20.9% |
반응 단계
A suspension of lithium aluminium hydride (3 g, 0.08 mols) in 350 ml of anhydrous ether is added with 0.5 g of 3-(2-hydroxy-5-methyl-phenyl)-N,N-diisopropyl-3-phenyl-propionamide in portions. The mixture is refluxed while stirring for 4 days. Afterwards, water is carefully added to destroy the lithium aluminium hydride excess, the mixture is acidified to pH 5 with acetic acid, the ether phase is separated and dried over sodium sulfate. The solvent is evaporated to obtain an oil which is purified by flash chromatography (eluent hexane-ethyl acetate 7:3). 0.1 g of tolterodine free base are obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07420091B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-dcfc5940852349d2a6c25acb5c3b04d2 |
| 출처 메모 | uspto-grants-2008_09 |