Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Benzo(B)Thiophene → 2-[2-(4-Hydroxy-4-(2-benzothienyl)-piperidino)-ethyl]-1,4-benzodioxan
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Benzo(B)Thiophene | HCID 7221 | — |
| 반응물 | Diisopropylamine | HCID 7912 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | Lithium diisopropylamide | HCID 2724682 | — |
| 반응물 | 1-[2-(2,3-Dihydro-1,4-benzodioxin-2-yl)ethyl]piperidin-4-one | HCID 20540170 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Hexane | HCID 8058 | — |
| 생성물 | 2-[2-(4-Hydroxy-4-(2-benzothienyl)-piperidino)-ethyl]-1,4-benzodioxan | HCID 53672426 | — |
반응 단계
To lithium diisopropylamide in 50 ml of tetrahydrofuran, prepared from 2.25 ml of diisopropylamine and 10 ml of 1.6 N n-butyl lithium in hexane at -70° under nitrogen, is added 2.0 g of thianapthene in 20 ml of tetrahydrofuran while stirring. After 1 hour, the solution of 2.65 g of 2-[2-(4-oxopiperidino)-ethyl]-1,4-benzodioxan in 20 ml of tetrahydrofuran is added and, after standing overnight, the mixture is decomposed with 9 ml of saturated aqueous ammonium chloride. The organic phase is separated, dried, evaporated, the crystalline residue washed with water and recrystallized from ethanol-acetone, to yield the 2-[2-(4-hydroxy-4-(2-benzothienyl)-piperidino)-ethyl]-1,4-benzodioxan melting at 175°-178°.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04129655 |
| 출처 데이터셋 | uspto-grants-1978_12 |
| ORD ID | ord-1e59a395996d4453b46b92702fa9db02 |
| 출처 메모 | uspto-grants-1978_12 |