참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Hydrazine, (4-chlorophenyl)-, hydrochloride (1:1) | HCID 71600 | — |
| 반응물 | 1-(4,6-Dimethoxypyrimidin-2-yl)propan-2-one | HCID 11264052 | — |
| 촉매 | Zincchloride | HCID 3007855 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 5-Chloro-3-(4,6-dimethoxypyrimidine-2-yl)-2-methylindole | HCID 17856766 | 84% |
반응 단계
To 80 ml of toluene were added 8.0 g (40 m moles) of 1-(4,6-dimethoxypyrimidine-2-yl)-2-propanone and 7.9 g (44 m moles) of 4-chlorophenylhydrazine hydrochloride. Thereto was added 6.54 g (48 m moles) of zinc chloride. Refluxing was made for 2 hours with heating. The reaction mixture was allowed to cool. Then, ethyl acetate and water were added to dissolve the whole reaction mixture. The organic layer was washed with water, separated, and dried over Glauber's salt. The resulting organic layer was concentrated under reduced pressure using a rotary evaporator to obtain an orange solid. The solid was washed with isopropyl ether to obtain 10.2 g (33.7 m moles) of 5-chloro-3-(4,6-dimethoxypyrimidine-2-yl)-2-methylindole. Yield: 84% Melting point: 179 to 181° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07531654B2 |
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| 출처 데이터셋 | uspto-grants-2009_05 |
|---|
| ORD ID | ord-ead58d8be5a34a75b626e3cf4bce05b5 |
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| 출처 메모 | uspto-grants-2009_05 |
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