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Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 971830생성일: 2026년 10월 25일

Ammonia → 3,3,6,6,9,9-Hexamethyl-1,2,4,5-tetraoxa-3-silacyclononane

https://huagongshe.com/reaction/971830

반응식

참여 물질

역할이름HCID투입량
반응물AmmoniaHCID 222—
반응물DichlorodimethylsilaneHCID 6398—
반응물2,5-Dimethylhexane 2,5-dihydroperoxideHCID 520470—
용매Diethyl EtherHCID 3283—
생성물3,3,6,6,9,9-Hexamethyl-1,2,4,5-tetraoxa-3-silacyclononaneHCID 2131191962.4%

반응 조건

온도5 °C

반응 단계

Into a one liter flask equipped with a motorized stirrer is added 0.15 mole (25.17g, 98.47% pure) of 2,5-dimethyl-2,5-dihydroperoxyhexane and 0.15 mole (19.35g) of dichlorodimethylsilane in 400 ml of anhydrous ether. This mixture is cooled to about 5° C., and ammonia gas is introduced cautiously. Reaction temperature is maintained between 5° and 10° C. by use of an ice bath and by adjusting the rate of gas introduction. Ammonia addition is continued for 30 to 40 minutes until the exothermic reaction has stopped. The reaction mixture is then stirred at room temperature for an additional 3 hours. The salts are removed by filtration and the ether is removed by distillation. The crude yield of a colorless solid was 26.7 grams. To purify the crude product hexane is added and the mixture is filtered to remove a small amount of insoluble, unreacted 2,5-dimethyl-2,5-dihydroperoxyhexane. Evaporation of the hexane yields 21.9 grams (62.4%) of 3,3,6,6,9,9-hexamethyl-1,2,4,5-tetraoxa-3-silacyclononane having a melting point of 44.5°-48° C. The product is 95.5% pure based upon active oxygen (A.O.) analysis wherein theoretical A.O. is 13.67% and A.O. found is 13.05%. Analysis of the product supports the structure ##STR4## as follows: (1) I.R. spectrum indicates no terminal hydroperoxy (--OOH) groups; (2) the molecular weight corresponds to a cyclic structure; and (3) various chromatographic analyses verify a very non-polar species.

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US04161485
출처 데이터셋uspto-grants-1979_07
ORD IDord-9c561966ae6b4c559e70d10e6c601d93
출처 메모uspto-grants-1979_07