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Potassium Carbonate → 2-(3,4,4-Trifluoro-1-oxo-3-butenyl)amino-4,6-dimethoxy-pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Amino-4,6-dimethoxypyrimidine | HCID 118946 | — |
| 反応物 | 3,4,4-Trifluoro-3-butenoyl chloride | HCID 10920789 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(3,4,4-Trifluoro-1-oxo-3-butenyl)amino-4,6-dimethoxy-pyrimidine | HCID 15335027 | 10.7% |
反応手順
To an ice-cooled stirred suspension of 2-amino-4,6-dimethoxypyrimidine (1.55 g, 10 mmol) in dichloromethane (50 mL) and potassium carbonate (2.76 g, 20 mmol) in water (20 mL) was added 3,4,4-trifluoro-3-butenoyl chloride (3.17 g, 20 mmol). The reaction mixture was stirred in cold for 10 min and at r.t. for 15 min. The organic layer was washed with 3N HCl (2×25 mL), saturated sodium bicarbonate (25 mL) and brine, and dried. Evaporation of the solvent gave 0.296 g (10%) of the title compound as a white solid. m.p. 127°-130° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05723470 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-7acdd14915da464f89faabd34f59b6eb |
| 出典メモ | uspto-grants-1998_03 |