참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | o-Tolylhydrazinium(1+) chloride | HCID 71554 | — |
| 반응물 | 1-(4,6-Dimethoxypyrimidin-2-yl)propan-2-one | HCID 11264052 | — |
| 촉매 | Zincchloride | HCID 3007855 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Ethyl acetate hexane | HCID 21226206 | — |
| 생성물 | 3-(4,6-Dimethoxypyrimidine-2-yl)-2,7-dimethylindole | HCID 12979370 | 34.2% |
반응 단계
In 20 ml of toluene were dissolved 0.77 g (3.9 m moles) of 1-(4,6-dimethoxypyrimidine-2-yl)-2-propanone and 0.69 g (4.3 m moles) of 2-methylphenylhydrazine hydrochloride. Thereto was added 0.64 g (4.7 m moles) of zinc chloride, followed by refluxing for 2 hours. The reaction mixture was allowed to cool, and then ethyl acetate and water were added to dissolve the whole reaction mixture. The oily layer was washed with water, separated and dried over Glauber's salt. The resulting oily layer was concentrated under reduced pressure using a rotary evaporator, to obtain an orange solid. The solid was treated with ethyl acetate/n-hexane to obtain 0.38 g (1.34 m moles) of 3-(4,6-dimethoxypyrimidine-2-yl)-2,7-dimethylindole. Yield: 34% Melting point: 145 to 147° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07504503B2 |
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| 출처 데이터셋 | uspto-grants-2009_03 |
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| ORD ID | ord-1a9c4ecc38a444a3819090779b3e6868 |
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| 출처 메모 | uspto-grants-2009_03 |
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