참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Fluorene | HCID 6853 | — |
| 반응물 | Acetic Anhydride | HCID 7918 | — |
| 반응물 | Aluminum(III) Chloride | HCID 6451240 | — |
| 용매 | Chlorobenzene | HCID 7964 | — |
| 생성물 | 2-Acetylfluorene | HCID 69908 | — |
반응 단계
Fluorene is acylated by acetic anhydride in an organic solvent, e.g., chlorobenzene in the presence of aluminum chloride at 18°-20° C at the initial stage of the process followed by heating to 40°-50° C to obtain 2-acetylfluorene at a yield of up to 74 weight percent. The latter is oxidized by chromic acid or by the salts thereof in an acetic acid medium at 50°-90° C for 4-12 hours to obtain 2-acetylfluorenone in a yield of 27-68 weight percent as calculated for 2-acetylfluorene, or 20-50 weight percent when calculated for fluorene. The resultant product is brominated in an organic solvent, e.g., chloroform at 50°-60° C or in acetic acid at 100°-110° C. The yield of the thus-formed 2-ω-dibromoacetylfluorenon equals 71-88 weight percent as calculated for 2-acetylfluorenone, or 35.4-44 weight percent when calculated for fluorene. Then 2-ω-dibromoacetylfluorenone is made to react with morpholine when heated to 50°-98° C for 1-2 hours to obtain 2-ω-bismorpholinoacetylfluorenone in a yield of 40-85 weight percent as calculated for 2-ω-dibromoacetylfluorenone, or 17.6-37.4 weight percent when calculated for fluorene.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04016289 |
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| 출처 데이터셋 | uspto-grants-1977_04 |
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| ORD ID | ord-83684ae7b94c42b3a73aaf000530d66e |
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| 출처 메모 | uspto-grants-1977_04 |
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