Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Formaldehyde → 5,11-Dihydro-11-[1-oxo-6-(1-piperidinyl)-4-hexynyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Formaldehyde | HCID 712 | — |
| 반응물 | Piperidine | HCID 8082 | — |
| 반응물 | 5,11-dihydro-11-[1-oxo-4-pentynyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one | HCID 13729188 | — |
| 촉매 | Cuprous chloride | HCID 62652 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 5,11-Dihydro-11-[1-oxo-6-(1-piperidinyl)-4-hexynyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one | HCID 13729189 | — |
반응 단계
A mixture consisting of 9.6 g (0.03 mol) of 5,11-dihydro-11-[1-oxo-4-pentynyl]-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one, 1.08 g (0.036 mol) of paraformaldehyde, 3.06 g (0.036 mol) of piperidine, 0.2 g of copper(I) chloride and 150 ml of dioxan is refluxed for 1 hour. After the reaction has ended the insoluble constituents are filtered off and the filtrate is evaporated to dryness in vacuo. The crude product is purified by column chromatography on silica gel (mobile phase: ethyl acetate, ethyl acetate+10% methanol). After recrystallisation from ethyl acetate, 2.7 g (21% of theory) of the desired compound are obtained, m.p. 197° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04724236 |
| 출처 데이터셋 | uspto-grants-1988_02 |
| ORD ID | ord-301ed65de99248bebe2bd6e6ac674570 |
| 출처 메모 | uspto-grants-1988_02 |