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1,1,1-Trifluoro-2-methylpropan-2-ol → 4-Nitrophenyl 1,1,1-Trifluoro-2-Methylpropan-2-yl-carbonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,1,1-Trifluoro-2-methylpropan-2-ol | HCID 68182 | — |
| 反応物 | 4-Nitrophenyl chloroformate | HCID 82129 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-Nitrophenyl 1,1,1-Trifluoro-2-Methylpropan-2-yl-carbonate | HCID 57785183 | — |
反応手順
To a solution of 1,1,1-trifluoro-2-methylpropan-2-ol (1.0 g) in THF (30 mL) was added a 2M solution of n-butyl lithium in n-hexane (3.9 mL) and then 4-nitrophenyl chloroformate (2.4 g) at −75° C. The mixture was warmed to room temperature and diluted with ethyl acetate, washed with water, dried over sodium sulfate, filtered and concentrated in vacuo. The residue was purified by silica gel chromatography (0-50% EtOAc/Hexane) to give 4-nitrophenyl 1,1,1-trifluoro-2-methylpropan-2-yl carbonate as a pale yellow foam.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08263632B2 |
| 出典データセット | uspto-grants-2012_09 |
| ORD ID | ord-3bf51f7a5c41482e8f8af026c33c8c4c |
| 出典メモ | uspto-grants-2012_09 |