化工社化工社 化学情報印刷レポート · 研究参考用
Sodium hydride → 2-butyl-3-[4-[(1-carbomethoxy) (1-phenyl)methoxy]-3-chlorophenyl]methyl-6-methylquinazolin-4(3H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Methyl 2-(2-chloro-4-bromomethylphenoxy)-2-phenylacetate | HCID 19385604 | — |
| 反応物 | HCID 178441839 | HCID 178441839 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-butyl-3-[4-[(1-carbomethoxy) (1-phenyl)methoxy]-3-chlorophenyl]methyl-6-methylquinazolin-4(3H)-one | HCID 19934853 | 52.4% |
反応手順
To a half suspension of 62 mg (0.287 mmol) of the product of Step A of Example 1 in 1.0 mL of anhydrous DMF was added 12 mg (1.05 eq) of a 60% oil dispersion of sodium hydride and the reaction mixture was stirred under an N2 atmosphere. After stirring 10 minutes at room temperature, a solution of 0.127 g (1.2 eq) of the product of Step B dissolved in 1.0 mL DMF was added to the solution of the anion. The reaction mixture was then stirred overnight, then partitioned between water and ethyl acetate. The organic layer was separated, dried (MgSO4), filtered and evaporated in vacuo. The residual oil was purified on a silica gel flash chromatography column eluted with 30% ethyl acetate/hexane to afford 76 mg (52%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05264439 |
| 出典データセット | uspto-grants-1993_11 |
| ORD ID | ord-39e927e176c74d328f5c9169e3bed87a |
| 出典メモ | uspto-grants-1993_11 |