関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Pivalaldehyde | HCID 12417 | — |
| 反応物 | 3-Thiazolidineacetic acid, 4-oxo-2-thioxo- | HCID 79793 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Carboxymethyl-5-(2,2-dimethylpropylidene)rhodanine | HCID 54444689 | 62.7% |
反応手順
Into 20 ml of dry DMF was dissolved 1.5 g (0.008 mole) of 3-carboxymethylrhodanine. To the solution was added 2.2 g (0.016 mole) of K2CO3 at a room temperature, and further 1 g (0.012 mole) of 2,2-dimethylpropanal was added dropwise at 60° C. After agitating at 60° C. for 30 minutes, the reaction mixture was poured into water. The resultant was adjusted to pH 4 with a dilute hydrochloric acid and then extracted with ethyl acetate. The extract was purified through a silica gel column and recrystallized from a mixed solvent of ethyl acetate and ethanol to give 1.3 g of 3-carboxymethyl-5-(2,2-dimethylpropylidene)rhodanine in the form of light yellow needle (yield: 63%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04609736 |
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| 出典データセット | uspto-grants-1986_09 |
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| ORD ID | ord-7c6c6c5c2879429d939127f5a9ef0417 |
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| 出典メモ | uspto-grants-1986_09 |
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