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Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 1796889생성일: 2026년 10월 27일

Sodium Iodide → Silane, trimethyl[[2-methyl-1-(1-methylethyl)-1-propenyl]oxy]-

https://huagongshe.com/reaction/1796889

반응식

참여 물질

역할이름HCID투입량
반응물Sodium IodideHCID 5238—
반응물AcetonitrileHCID 6342—
반응물ChlorotrimethylsilaneHCID 6397—
반응물2,4-Dimethyl-3-pentanoneHCID 11271—
용매TriethylamineHCID 8471—
생성물Silane, trimethyl[[2-methyl-1-(1-methylethyl)-1-propenyl]oxy]-HCID 1109532796.6%

반응 단계

Acetonitrile (300 mL) was mixed with 20.3 g of diisopropyl ketone, 32 g of sodium iodide, and 21.6 g of triethylamine, to which was gradually added 23.1 g of chlorotrimethylsilane. The mixed solution was reacted at 50° C. for 4 hours and then allowed to stand for cooling. The reaction mixture was poured into ice and extracted with hexane. An organic phase was rinsed with a sodium hydrogencarbonate solution, dried, and then concentrated. The resultant was purified by distillation in vacuo to obtain 32 g of 2,4-dimethyl-3-trimethylsilyloxy-2-pentene (silylenol ether of diisopropyl ketone). The resulting silylenol ether (15 g) and 8.8 g of tetramethylene sulfoxide were dissolved in 150 mL of chloroform under a nitrogen gas stream. The solution was cooled to −30° C. or lower, and 17.7 g of trifluoroacetic anhydride was added dropwise thereto over 30 minutes. The mixture was reacted at room temperature for 1 hour, and a solution of potassium nonafluorobutanesulfonate in acetonitrile/water was added to the reaction mixture. The mixture was extracted with chloroform, and an organic phase was subjected to alkali rinsing with a 5% by weight tetramethylammonium hydroxide aqueous solution, followed by rinsing with distilled water until aqueous phases had become neutral. An organic phase was concentrated, and diisopropyl ether was added to the resulting crude product to deposit a powder. The powder was collected by filtration to obtain 17 g of Compound (I-1).

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US07033727B2
출처 데이터셋uspto-grants-2006_04
ORD IDord-976b381f591f4c2da3d4475b0772bb50
출처 메모uspto-grants-2006_04