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Tetrahydrofuran → HCID 178496595、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | HCID 178496608 | HCID 178496608 | — |
| 生成物 | HCID 178496595 | HCID 178496595 | 67% |
反応手順
To a solution of 6-chloro-N4-(trans-4-methoxycyclohexyl)pyrimidine-2,4,5-triamine (5.5 g, 20.36 mmol) in 300 mL of anhydrous THF (use oven dried glassware) was added 1,1-carbonyldiimidazole (newly opened bottle, 19.8 g, 122.2 mmol, 6 equiv.) as a solid, in portions. The reaction mixture was stirred at room temperature for 2 h (completion of the reaction checked by HPLC and MS). The solvent was removed in vacuo. Water (250 mL) was added to the residue and the mixture stirred at room temperature for 10 min. The solid formed was filtered under vacuum, washed with cold water and thoroughly dried to give the desired product as a brown solid (67% yield), which was used in the next step without further purification. MS (EI) m/z 298 (MH)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07902187B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-22eda96e103b4c079ebe3ad8db13d2b3 |
| 出典メモ | uspto-grants-2011_03 |