関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Amino-4-(trifluoromethyl)benzenethiol hydrochloride | HCID 2734678 | — |
| 反応物 | 3-Fluoroisonicotinaldehyde | HCID 2763003 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(3-Fluoropyridin-4-yl)-5-(trifluoromethyl)benzothiazole | HCID 67113761 | 60.1% |
反応手順
A mixture of 2.3 g of 2-amino-4-(trifluoromethyl)-benzenethiol hydrochloride, 1.25 g of 3-fluoroisonicotinaldehyde, 1.29 g of N-ethyldiisopropylamine and 10 ml of DMSO was stirred for 5 hours at 170° C. The reaction mixture was cooled down to room temperature. To the reaction mixture was added water, and the resultant mixture was extracted with ethyl acetate twice. The combined organic layers were washed with water and saturated saline, dried over magnesium sulfate, then, concentrated under reduced pressure. The residue was subjected to silica gel column chromatography, to obtain 1.79 g of 2-(3-fluoropyridin-4-yl)-5-(trifluoromethyl)benzothiazole (hereinafter, referred to as the present compound 1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08742112B2 |
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| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-81783412adec46318b8f5c9a7909478f |
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| 出典メモ | uspto-grants-2014_06 |
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