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HRID 376825생성일: 2026년 10월 26일

Stannane, chlorotricyclohexyl- → Tricyclohexyl [o-(1-hydroxyethyl)phenyl]tin

https://huagongshe.com/reaction/376825

반응식

참여 물질

역할이름HCID투입량
반응물Stannane, chlorotricyclohexyl-HCID 76539—
반응물1-(2-Bromophenyl)ethanolHCID 95455—
반응물ButyllithiumHCID 178418339—
용매WaterHCID 962—
용매Diethyl EtherHCID 3283—
용매HexaneHCID 8058—
생성물Tricyclohexyl [o-(1-hydroxyethyl)phenyl]tinHCID 1935951273%

반응 조건

온도-30 °C

반응 단계

10.1 g of o-bromo-1-phenylethanol (50.2 mmol) and 50 ml of diethylether were mixed together in a 500 ml two-neck flask, which was equipped with a stirrer and isobaric dropping funnel. To this mixture, 64.5 ml of hexane solution of n-butyl lithium was gradually added dropwise at -78° C. Subsequently, the temperature was raised to -30° C., and the mixture was stirred for 1 hour while maintaining the same temperature. The reaction mixture was cooled back to -78° C., and a mixed solvent solution containing 20.2 g of tricyclohexyltin chloride (50.1 mmol), 100 ml of hexane, and 50 ml of diethylether was added dropwise thereto. The temperature was raised back to -30° C., and the mixture was stirred for 12 hours at the same temperature. Upon completion of the reaction, 100 ml of water was added, and the organic substance was extracted three times, with 200 ml of diethylether for each. After the solvent was removed under reduced pressure, the oily product was purified by column chromatography on silica gel (for which, 50 g of silica gel, and a mixed solvent of hexane and diethylether, as a developing solvent, were employed) to yield 17.9 g of the final product (yield=73.0%).

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US06022822
출처 데이터셋uspto-grants-2000_02
ORD IDord-dc7c027c1dee4fd7a5af4337fbe8a0f9
출처 메모uspto-grants-2000_02