関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Hydroxy-2-(trifluoromethyl)thiophene | HCID 11084273 | — |
| 反応物 | HCID 12115990 | HCID 12115990 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 11524380 | HCID 11524380 | 59% |
反応手順
A mixture of 0.4 g (1.24 mmol) of 5-methoxy-4-methylsulfonyl-2-(4-trifluoromethyl-1H-1-pyrazolyl)pyrimidine, 0.27 g (1.60 mmol) of 3-hydroxy-5-trifluoromethyl-thiophene and 0.34 g (2.47 mmol) of K2CO3 in 10 ml of DMF is stirred at 60° C. for 6 h and then at RT for 48 h. It is subsequently poured into 20 ml of water and extracted with four times 15 ml of CH2Cl2. The combined organic phase is dried over Na2SO4, filtered and concentrated. Chromatographic purification on silica gel with heptane/ethyl acetate (3:7) as eluent gives 0.3 g of 5-methoxy-2-(4-trifluoromethyl-1H-1-pyrazolyl)-4-(5-trifluoromethyl-3-thienyloxy)pyrimidine as colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07211673B2 |
|---|
| 出典データセット | uspto-grants-2007_05 |
|---|
| ORD ID | ord-c1671ce1ad6b441c8f8873f2c82ce678 |
|---|
| 出典メモ | uspto-grants-2007_05 |
|---|
