関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Bromo-1,1,2-trifluorobut-1-ene | HCID 66333 | — |
| 反応物 | Ammonium dithiocarbamate | HCID 11083854 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3,4,4-Trifluoro-3-butenyl dithiocarbamate | HCID 11298598 | — |
反応手順
2.8 g (25 mmol) of ammonium dithiocarbamate in 40 ml of ethanol are admixed dropwise with 5.32 g (26.3 mmol; purity 93.2%) of 4-bromo-1,1,2-trifluoro-1-butene, stirred at 40° C. for 3 h, another 2.8 g of ammonium dithiocarbamate is added after 1 h, and everything is left to stand at room temperature for 8 h. The filtrate is filtered off with suction and concentrated by evaporation under reduced pressure, the residue taken up in dichloromethane and washed once with water, and the organic phase dried over sodium sulphate. After concentration by evaporation under reduced pressure, 4.3 g (63% of theory; purity by GC/MS: 74 area %) of a semicrystalline residue are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07439408B2 |
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| 出典データセット | uspto-grants-2008_10 |
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| ORD ID | ord-a799ba5cb39d4e0b8ea74c4cb6b7d939 |
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| 出典メモ | uspto-grants-2008_10 |
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