참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Chloroacetyl chloride | HCID 6577 | — |
| 반응물 | Benzene, 2,4-dimethoxy-1-methyl- | HCID 96403 | — |
| 반응물 | Aluminum(III) Chloride | HCID 6451240 | — |
| 촉매 | Zincchloride | HCID 3007855 | — |
| 용매 | 1,2-Dichloroethane | HCID 11 | — |
| 생성물 | 1-(2,4-Dimethoxy-5-methylphenyl)-2-chloro-1-ethanone | HCID 19028015 | — |
반응 단계
A suspension of 5.24 g of AlCl3 and 0.52 g of ZnCl2 in 40 ml of 1,2-dichloroethane is cooled to 0° C., and a solution of 5.0 g of 2,4-dimethoxytoluene in 20 ml of 1,2-dichloroethane is added dropwise. The mixture is then cooled to -10° C., and a solution of 2.9 ml of chloroacetyl chloride in 1.5 ml of 1,2-dichloroethane is added dropwise while the temperature of the reaction medium is maintained at between -10° C. and -7° C. The mixture is left stirring while the temperature is allowed to rise to r.t., the reaction medium is poured into a mixture of ice and concentrated HCl, the resulting mixture is extracted with DCM, the combined organic phases are washed with water and dried over magnesium sulphate and the solvents are evaporated off under vacuum. The residue is taken up in heptane and the precipitate formed is filtered off. 3.0 g of the expected product, m.p.=166°-167° C., are obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05656648 |
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| 출처 데이터셋 | uspto-grants-1997_08 |
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| ORD ID | ord-e80e0e360fcb46a1a35cd7976d080b65 |
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| 출처 메모 | uspto-grants-1997_08 |
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