참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | O-Cresol | HCID 335 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Fluoreneone | HCID 22281833 | — |
| 촉매 | 1-Dodecanethiol | HCID 8195 | — |
| 생성물 | 4,4'-(9H-Fluorene-9,9-diyl)bis(2-methylphenol) | HCID 11014345 | 156.9% |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08841491B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-eb66a1f238504bd7aa0d3e7dd26b20af |
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| 출처 메모 | uspto-grants-2014_09 |
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