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Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 1294574생성일: 2026년 10월 24일

Methylamine ethanol → 8-[2-(6,6-Dimethyl-bicyclo[3.1.1]hept-2-yl)-ethyl]-3-(3-methylamino-propyl)-1-phenyl-1,3,8-triaza-spiro[4.5]decan-4-one

https://huagongshe.com/ko/reaction/1294574

반응식

참여 물질

역할이름HCID투입량
반응물Methylamine ethanolHCID 22028356—
반응물3-(3-Chloro-propyl)-8-[2-(6,6-dimethyl-bicyclo[3.1.1]hept-2-yl)-ethyl]-1-phenyl-1,3,8-triaza-spiro[4.5]decan-4-oneHCID 58906443—
촉매Sodium IodideHCID 5238—
용매WaterHCID 962—
용매Ethyl AcetateHCID 8857—
생성물8-[2-(6,6-Dimethyl-bicyclo[3.1.1]hept-2-yl)-ethyl]-3-(3-methylamino-propyl)-1-phenyl-1,3,8-triaza-spiro[4.5]decan-4-oneHCID 1123633752.2%

반응 조건

온도70 °C

반응 단계

The crude spiro compound (23) (162.8 g; 0.36 mol) was dissolved in methylamine/EtOH solution (Fluka, 8M; 1154 ml; 9.23 mol). Sodium iodide (2.16 g; 0.014 mol) was added and the solution was stirred at 70° C. under N2-atmosphere for 3 days. After cooling the reaction mixture was diluted with water and EtOAc (500 ml each). The aqueous layer was extracted with EtOAc (3×800 ml). The organic layer was washed with brine (500 ml). After drying on Na2SO4 the solvent was evaporated to yield a yellow oil. This oil was purified by column chromatography (SiO2; CH2Cl2/MeOH 90:10; containing 1% 7N NH3/MeOH) to yield 30 g of (24) with a purity of 93% (according to HPLC/MS) and 85 g of (24) with a purity of 96% (115 g; 0.25 mol; 70%).

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US07241770B2
출처 데이터셋uspto-grants-2007_07
ORD IDord-9cab9986065f42eb9aadb90d095cd1d8
출처 메모uspto-grants-2007_07