Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Methyl-3-pyrrolidinol → 3-Butoxy-4-(1-methyl-pyrrolidin-3-yloxy)-[1,2,5]thiadiazole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Methyl-3-pyrrolidinol | HCID 93074 | — |
| 반응물 | 3-Butyloxy-4-methanesulfonyl-1,2,5-thiadiazole | HCID 19600307 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Hexane | HCID 8058 | — |
| 생성물 | 3-Butoxy-4-(1-methyl-pyrrolidin-3-yloxy)-[1,2,5]thiadiazole | HCID 10825055 | — |
반응 단계
A solution of 1-methyl-3-pyrrolidinol (0.6 g, 0.0059 mol) in THF (20 mL) was treated with 1.6M n-butyllithium in hexane (3.1 mL), 0.005 mol). To the solution was added 3-butyloxy-4-methanesulfonyl-1,2,5-thiadiazole (1.0 g, 0.0042 mol) and the reaction heated to reflux overnight. The solvent was evaporated, the residue acidified with cold 1N HCl, and the mixture extracted with ether. The aqueous fraction was made basic, extracted with EtOAc, and the extracts washed with water. The extracts were dried and the solvent evaporated to give a liquid. The HCl salt (0.7 g) crystallized from EtOAc, m.p. 157°-158° C. (Compound 28).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05646289 |
| 출처 데이터셋 | uspto-grants-1997_07 |
| ORD ID | ord-08d74c03007f48d48c00e453ab59cd9a |
| 출처 메모 | uspto-grants-1997_07 |