참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Cyclohexanol | HCID 7966 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Carbonochloridic acid, cyclohexyl ester | HCID 83262 | — |
| 반응물 | Fenridazon | HCID 197225 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Hexane | HCID 8058 | — |
| 생성물 | Cyclohexyl 1-(4-chlorophenyl)-1,4-dihydro-4-oxo-6-methylpyridazine-3-carboxylate | HCID 13084122 | 65% |
반응 단계
To an ice cooled suspension of 5.29 g (0.02 mol) 1-(4-chlorophenyl)-1,4-dihydro-4-oxo-6-methyl pyridazine-3-carboxylic Acid (see Example 12) and 2.02 g (0.02 mol) of triethylamine in 75 ml of toluene there is added 3.25 g (0.02 mol) of cyclohexyl chloroformate. The suspension formed is stirred at room temperature for 15 minutes and to it there is added 3.2 g (0.022 mol) of cyclohexanol in 50 ml of toluene. The mixture is stirred at room temperature for 38 hrs. and to it there is added 100 ml of water. The mixture is stirred at room temperature for 1 hr. and the toluene layer is isolated and poured into 600 ml of hexane. The suspension formed is stirred at room temperature for 1/2 hr. and is vacuum filtered. The filter cake is air dried to afford 4.5 g (65% yield) of product, mp 160°-162° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04345934 |
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| 출처 데이터셋 | uspto-grants-1982_08 |
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| ORD ID | ord-1ff062a96b93482eaad2b50dc2687f39 |
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| 출처 메모 | uspto-grants-1982_08 |
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