참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | 4-Chlorobenzhydrol | HCID 8401 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | HCID 178516071 | HCID 178516071 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 5-(4-Chlorophenyl-phenylmethyl)-2-pyridone | HCID 22748799 | — |
반응 단계
Combine 109.3 g. (0.5 mole) of 4-chlorobenzhydrol with 142.7 g. (1.5 mole) of 2-hydroxypyridine and heat at 150° C. with stirring until molten. Add about 2 ml. of concentrated sulfuric acid and continue heating to 240°-250° C. while removing water from the reaction mixture. Permit the reaction to continue for about 2 hours, then cool the reaction mixture to about 25° C. Treat the resulting solid with ethyl acetate and water and filter to remove the undesired 3-(4-chlorophenyl-phenylmethyl)-2-pyridone. The organic layer is separated and washed with water several times and dried over potassium carbonate and filtered. Concentrate the filtrate to half volume and filter to remove the remaining 3-substituted-2-pyridone. Evaporate the filtrate and dissolve the residue in ethyl ether. Upon standing overnight the 5-(4-chlorophenyl-phenylmethyl)-2-pyridone crystallizes, yield 60 g., m.p. 164°-169° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04138488 |
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| 출처 데이터셋 | uspto-grants-1979_02 |
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| ORD ID | ord-072bd13939bc4688af71208be225f59c |
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| 출처 메모 | uspto-grants-1979_02 |
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