Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Iodide → 8-[3-[4-(3-Methylphenyl)-1-piperazinyl]propyloxy]-8-azaspiro[4.5]decan-7,9-dione hydrochloride hemihydrate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Iodide | HCID 5238 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 1-(m-Tolyl)piperazine dihydrochloride | HCID 83110 | — |
| 반응물 | 8-(3-Bromopropyloxy)-8-azaspiro[4.5]decan-7,9-dione | HCID 14280583 | — |
| 촉매 | Tetrabutylammonium Bromide | HCID 74236 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 생성물 | 8-[3-[4-(3-Methylphenyl)-1-piperazinyl]propyloxy]-8-azaspiro[4.5]decan-7,9-dione hydrochloride hemihydrate | HCID 131715932 | — |
반응 단계
A mixture of 8-(3-bromopropyloxy)-8-azaspiro[4.5]decan-7,9-dione (5.0 g), 1-(3-methylphenyl)piperazine dihydrochloride (4.11 g), K2CO3 (9.1 g), NaI (100 mg) and n-Bu4NBr (100 mg) in 100 ml of dry tolune was heated at 80° with stirring under N2. After 4 hours, 50 ml of CH3CN was added. Heating was continued for 18 hr. and 5 ml of Et3N was added. Heating was continued for an additional 6 hr and at which time no starting material remained by TLC. The mixture was cooled to room temperature and filtered. The solvents were removed in vacuo and the residue was chromatographed on silica using ethyl acetate as the eluent. The fractions containing the desired product were combined and concentrated in vacuo.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04826846 |
| 출처 데이터셋 | uspto-grants-1989_05 |
| ORD ID | ord-1130f591a1a14fe580015499fe06b735 |
| 출처 메모 | uspto-grants-1989_05 |