関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | N,N-Dimethylethylenediamine | HCID 66053 | — |
| 反応物 | ((4-Bromo-2-fluorobenzyl)oxy)(tert-butyl)dimethylsilane | HCID 57685175 | — |
| 溶媒 | Ammonia | HCID 222 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | tert-Butyl-(2-fluoro-4-iodo-benzyloxy)-dimethyl-silane | HCID 67007573 | — |
反応手順
To 7.70 g (24.1 mmol) (4-bromo-2-fluoro-benzyloxy)-tert-butyl-dimethyl-silane (preparation 16a) in 8 mL 1,4-dioxane is added 937 mg (4.82 mmol) Cu(I)-iodide. The reaction mixture is flushed with argon and 7.23 g (48.2 mmol) sodium iodide and 1.03 mL (9.65 mmol) N,N-dimethylethylen-diamine are added. The mixture is stirred at 120° C. for 7 h in a sealed tube. The reaction mixture is diluted at RT with 5% aqueous NH3-solution and the aqueous phase is extracted with EtOAc. The combined organic phase is washed a few times with water, dried over MgSO4, filtered and the solvent is evaporated.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08067590B2 |
|---|
| 出典データセット | uspto-grants-2011_11 |
|---|
| ORD ID | ord-a2ddbe30031644f98d7896cc62d2e042 |
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| 出典メモ | uspto-grants-2011_11 |
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