関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3,5-Dimethyl-4-hydroxybenzonitrile | HCID 20176 | — |
| 反応物 | 1-Pentyne, 5-chloro- | HCID 84308 | — |
| 溶媒 | 1-Methylpyrrolidine | HCID 8454 | — |
| 生成物 | Benzonitrile, 3,5-dimethyl-4-(4-pentynyloxy)- | HCID 10059076 | — |
反応手順
A mixture of 40 g 3,5-dimethyl-4-hydroxybenzonitrile, 32 ml 5-chloro-1-pentyne (d=0.968) and 74.63 g milled potassium carbonate in 25 ml N-methylpyrrolidine was heated under nitrogen at 100° C. with stirring for four hours. The mixture, after cooling to room temperature and addition of 300 ml water, was extracted with ethyl acetate. The ethyl acetate extracts were washed with aqueous 2N sodium hydroxide solution and saturated sodium chloride solution, dried (MgSO4) and then concentrated in vacuo. The residue was subjected to flash filtration (activated magnesium silicate; ether/hexane) and the filtrate was concentrated in vacuo to give, after recrystallization (methyl alcohol/0° C.) 34.64 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05175177 |
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| 出典データセット | uspto-grants-1992_12 |
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| ORD ID | ord-8dc7b6e04ba64a2cbe75d6b15672e699 |
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| 出典メモ | uspto-grants-1992_12 |
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