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Tetrahydrofuran → N-(3-Amino-4-thienyl)-N'-(2,6-dichlorophenyl)thiourea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 1,3-Dichloro-2-isothiocyanatobenzene | HCID 123239 | — |
| 反応物 | 3,4-Diaminothiophene dihydrochloride | HCID 12707342 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-(3-Amino-4-thienyl)-N'-(2,6-dichlorophenyl)thiourea | HCID 86037735 | — |
反応手順
A mixture of 1.87 g of 3,4-diaminothiophene dihydrochloride, 60 ml of anhydrous THF and 2.58 g of N-ethyl-N,N-diisopropylamine was stirred at room temperature for 30 minutes and then admixed with 2.04 g of 2,6-dichlorophenyl isothiocyanate. After the mixture had been heated to 40° C. for 10 minutes, it was stirred at room temperature for approx. 18 hours, and the solvent was distilled off, and the residue admixed with water and extracted repeatedly with ethyl acetate. After the combined organic phases had been treated with activated carbon, they were dried over sodium sulfate and the solvent was again distilled off. A crystalline solid was obtained and, after stirring with a little ethyl acetate, was filtered off. M.p. 165° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07179830B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-241168cd9bac4a46b0fa26436f3bd4f8 |
| 出典メモ | uspto-grants-2007_02 |