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Water → 5-(4-Nitrophenyl)thieno[2,3-d]pyrimidine-2,4-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Chloroformamidinium chloride | HCID 3084509 | — |
| 反応物 | 2-Amino-4-(4-nitrophenyl)thiophene-3-carbonitrile | HCID 15606113 | — |
| 溶媒 | Diglyme | HCID 8150 | — |
| 生成物 | 5-(4-Nitrophenyl)thieno[2,3-d]pyrimidine-2,4-diamine | HCID 69063045 | — |
反応手順
A suspension of Example 58B (1 g, 4.08 mmol) and chloroformamidine hydrochloride (1.17 g, 10.2 mmol) in diglyme (40 mL) was heated to 130° C. for 15 hours. The mixture was cooled to room temperature, diluted with water, and extracted twice with ethyl acetate. The combined extracts were washed with brine, dried (MgSO4), filtered, and concentrated. The residue was further concentrated under a stream of nitrogen, and purified by silica gel chromatography with 5 to 7% methanol/dichloromethane to provide 0.26 g of the desired product. MS (ESI(+)) m/e 288 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07560552B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-f20ae985763d49b29e6997f2e3bf926d |
| 出典メモ | uspto-grants-2009_07 |