関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Monomethyl phthalate | HCID 20392 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | (Z)-4-hydrazinyl-4-oxobut-2-enoic acid | HCID 12898265 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | HCID 178497632 | HCID 178497632 | — |
反応手順
Into a 100 ml round-bottomed flask fitted with a stirrer and reflux condenser there was charged 10.8 g (0.06 mole) of 2-carbomethoxybenzoic acid and 50 ml of chloroform. There was then added 7.8 g (0.066 mole) of SOCl2, followed by refluxing for 2 hr. The chloroform was then removed by distillation, followed by addition of 50 ml. of dimethoxyethane, 4.7 g (0.06 mole) of pyridine and 6.7 g (0.06 mole) of maleic hydrazide. The mixture was allowed to stir over night. The resulting reaction mixture was filtered to remove solids. Then the product was precipitated from the filtrate by addition of water and was recovered as a solid by filtration. The solid material was washed with hexane-ether solvent mixture and was filtered and dried. The yield was 6.6 g, m.p. 144°-145° C. Infrared and nuclear magnetic resonance spectra were consistent with the structure of the compound as named above.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04314843 |
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| 出典データセット | uspto-grants-1982_02 |
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| ORD ID | ord-5397526d64404379a863e61deeb8a066 |
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| 出典メモ | uspto-grants-1982_02 |
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