関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Diethylamine | HCID 8021 | — |
| 反応物 | Tetrafluoroethylene | HCID 8301 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2(3H)-Thiazolimine, 5-methyl-3-[3-(trifluoromethyl)phenyl]- | HCID 11021546 | — |
| 生成物 | 2-Difluoroacetylimino-3(3-trifluoromethylphenyl)-5-methylthiazoline | HCID 11088983 | 65% |
反応手順
A solution of 2-imino-3-(3-trifluoromethylphenyl)-5-methylthiazoline (0.52 g, 2.0 mmol), diethylamine (0.44 g, 6.0 mmol), triethylamine (0.61 g, 6.0 mmol) in N,N-dimethylformamide (10 ml) charged in a reaction flask was reacted with tetrafluoroethylene in the flask atmosphere (0.70 g, 7.0 mmol), which was supplied from a balloon tothe flask, at 50° C. for 21 hours. After cooling to an ambient temperature, the reaction mixture was poured into ice-water, and extracted with ethyl acetate. The ethyl acetate layer was washed with water and then brine, and dried over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was subjected to silica gel column chromatography, which afforded 2-difluoroacetylimino-3(3-trifluoromethylphenyl)-5-methylthiazoline (0.44 g, 1.3 mmol, yield 65%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05484933 |
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| 出典データセット | uspto-grants-1996_01 |
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| ORD ID | ord-eab9f5699d8545f7aaed6d0e26a88c89 |
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| 出典メモ | uspto-grants-1996_01 |
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