関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 3-Bromo-1,1,1-trifluoro-2-propanone | HCID 79008 | — |
| 反応物 | 5-(Methoxymethyl)-1,3,4-thiadiazol-2-amine | HCID 660844 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | Imidazo (2,1-b)-1,3,4-thiadiazole, 2-(methoxymethyl)-6-(trifluoromethyl)- | HCID 67117085 | 47% |
反応手順
Bromotrifluoroacetone (478 g, 1.05 eq) is added on a suspension of 5-(methoxymethyl)-1,3,4-thiadiazol-2-amine a25 (346 g, 1 eq) in 1,2-dimethoxyethane (6 l) at 20° C. The reaction mixture is heated to 80° C. until maximum conversion (<24 h). Water (4 l) is added to the reaction mixture at 32° C. and the expected compound crystallized out of the reaction mixture. The crystalline suspension is cooled to 10° C. to complete the crystallization process, filtered and the crystalline precipitate is washed with water (1.5 l) to afford 266 g of pure 2-(methoxymethyl)-6-(trifluoromethyl)imidazo[2,1-b][1,3,4]thiadiazole a28.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08822508B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-517397c5837b4522bbf3990d126ad048 |
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| 出典メモ | uspto-grants-2014_09 |
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