関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Dimethyl Sulfone | HCID 6213 | — |
| 反応物 | Ethyl 2-amino-4-methylthiophene-3-carboxylate | HCID 521132 | — |
| 反応物 | Chloroformamidinium chloride | HCID 3084509 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178431879 | HCID 178431879 | 87.9% |
反応手順
A mixture of ethyl 2-amino-4-methylthiophene-3-carboxylate (2.0 g, 11.7 mmol), chloroformamidine hydrochloride (3.357 g, 29.0 mmol) and dimethylsulfone (5.489 g, 58.4 mmol) was heated at 135° C. for 45 minutes. Water was added and the mixture was cooled down to room temperature. An aqueous ammonia solution was added to adjust the solution to pH 9. The precipitate was filtered off, yielding the title compound (1.863 g) as a white powder. 13C NMR δ (75 MHz, DMSO-d6) 168.98, 159.12, 153.21, 133.26, 114.37, 110.81, 16.35. MS (m/z) 182 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09227984B2 |
|---|
| 出典データセット | uspto-grants-2016_01 |
|---|
| ORD ID | ord-c1695a9815aa42c2b10daecd926f3082 |
|---|
| 出典メモ | uspto-grants-2016_01 |
|---|
