関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Allyl bromide | HCID 7841 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ethyl 2-(2-tritylamino-4-thiazolyl)-2-hydroxyiminoacetate | HCID 6802348 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Ethyl 2-(2-tritylaminothiazol-4-yl)-2-allyloxyiminoacetate | HCID 54525939 | 86.4% |
反応手順
Allyl bromide (2.91 g.) was added dropwise to a stirred suspension of ethyl 2-(2-tritylaminothiazol-4-yl)-2-hydroxyiminoacetate (syn isomer, 10 g.), N,N-dimethylformamide (100 ml.) and potassium carbonate (4.54 g.) under ice cooling over 5 minutes, and stirred at the same temperature for 4 hours. After adding water (200 ml.) to the resultant solution, the solution was extracted with diethyl ether twice. The extract was washed with a saturated aqueous solution of sodium chloride and dried over magnesium sulfate. The solution was concentrated in vacuo, and the residue was triturated with a solution of n-hexane and diethyl ether. The precipitates were collected by filtration to give ethyl 2-(2-tritylaminothiazol-4-yl)-2-allyloxyiminoacetate (syn isomer, 9.4 g.), mp. 130° to 132° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04604456 |
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| 出典データセット | uspto-grants-1986_08 |
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| ORD ID | ord-f6ae51bda7fb46b397d45384ffc8a80b |
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| 出典メモ | uspto-grants-1986_08 |
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