関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | tert-Butyl bromoacetate | HCID 79177 | — |
| 反応物 | 1-(2,6-Difluorophenyl)ethan-1-one | HCID 83643 | — |
| 反応物 | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | 2(1H)-Pyrimidinone, tetrahydro-1,3-dimethyl- | HCID 81646 | — |
| 生成物 | tert-Butyl 4-(2,6-difluorophenyl)-4-oxobutyrate | HCID 21964547 | — |
反応手順
To a stirred solution of 2,6-Difluoroacetophenone (5 g, 32 mmol) in dry THF (40 ml) and DMPU (8 ml) was added a solution of lithium bis(trimethylsilyl)amide (1.0M, 45 ml) at 60° C. under argon. After stirring for 10 minutes at −60° C., tert-Butyl bromoacetate (6.99 g, 35.8 mmol) was added rapidly. The reaction mixture was stirred for an additional 10 minutes and then warmed to room temperature for 4 hours. The crude mixture was taken in EtOAc and washed with water and brine. The aqueous layer was extracted one more time with EtOAc. The combined organic layers were dried over Na2SO4, filtered, concentrated and purified by flash chromatography on a silica gel column (hex:ethyl acetate, 2:1) to provide the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06946491B2 |
|---|
| 出典データセット | uspto-grants-2005_09 |
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| ORD ID | ord-75c5547bbc3e4b39aeea5bb4d92c18bf |
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| 出典メモ | uspto-grants-2005_09 |
|---|
