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Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 78960생성일: 2026년 10월 24일

Hydrochloric Acid → 4,4'-(9H-Fluorene-9,9-diyl)bis(2-methylphenol)

https://huagongshe.com/ko/reaction/78960

반응식

참여 물질

역할이름HCID투입량
반응물Hydrochloric AcidHCID 313—
반응물O-CresolHCID 335—
반응물Sodium HydroxideHCID 14798—
반응물FluoreneoneHCID 22281833—
촉매1-DodecanethiolHCID 8195—
생성물4,4'-(9H-Fluorene-9,9-diyl)bis(2-methylphenol)HCID 11014345156.9%

반응 조건

온도50 °C

반응 단계

A reaction was carried out by (a) feeding 23 g of fluorenone, 1.3 g of dodecyl mercaptan, and 161.0 g of 2-methyl phenol into a 500 ml glass reactor vessel equipped with a stirrer, a condenser and a thermometer, (b) dropping 13.0 g of 35% hydrochloric acid to a mixture, and (c) stirring the mixture at 50° C. for 2 hours. The amount of remaining fluorenone was determined by HPLC, and found to be 0.1% or less. To an obtained reaction mixture liquid, 18.5 g of 29% sodium hydroxide aqueous solution was added, and thereafter 94.0 g of 2-methyl phenol was distilled away from an organic phase by concentration under reduced pressure. To an obtained concentrated liquid, 161 g of toluene and 23 g of water were added, and the mixture liquid was stirred at 80° C. Thereafter, an aqueous phase was separated and removed, and a target substance partitioned in the organic phase was recovered. The organic phase was further washed twice with 23 g of water, and cooled to 10° C. Then, precipitated crystals were subjected to filtration and drying to obtain 37.9 g of 9,9-bis(4-hydroxy-3-methylphenyl)fluorene (yield: 84.3%, LC purity: 99.3%). Obtained 9,9-bis(4-hydroxy-3-methylphenyl)fluorene was dissolved by heat at 230° C. for 2 hours. The 9,9-bis(4-hydroxy-3-methylphenyl)fluorene thus dissolved had a hue of 1 in Gardner. The total amount of toluene used in the production was 4.2 parts by weight relative to 1 part by weight of the 9,9-bis(4-hydroxy-3-methylphenyl)fluorene.

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US08841491B2
출처 데이터셋uspto-grants-2014_09
ORD IDord-eb66a1f238504bd7aa0d3e7dd26b20af
출처 메모uspto-grants-2014_09