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Sodium Formate → Tert-butyl (5-formyl-2-methoxybenzyl)carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Formate | HCID 2723810 | — |
| 反応物 | Tert-butyl (5-bromo-2-methoxybenzyl)carbamate | HCID 22926030 | — |
| 反応物 | HCID 178418416 | HCID 178418416 | — |
| 触媒 | Triphenylphosphine | HCID 11776 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Tert-butyl (5-formyl-2-methoxybenzyl)carbamate | HCID 22493931 | 75.1% |
反応手順
1.015 g of tertiary butyl N-(5-bromo-2-methoxybenzyl)carbamate, 45 mg of dichlorobis(triphenylphosphine) palladium (II), 330 mg of sodium formate and 17 mg of triphenyl phosphine were dissolved in anhydrous N,N-dimethylformamide and stirred at 110° C. for 2 hours in a carbon monoxide atmosphere. The reaction mixture was diluted with ethyl acetate, and successively washed with water and saturated aqueous sodium bicarbonate. The organic layer was dried over anhydrous magnesium sulfate and the solvent was evapoarated. The residue was purified by silica gel column chromatography, and from fractions eluted with hexane-ethyl acetate (3:1), 640 mg of tertiary butyl N-(5-formyl-2-methoxybenzyl)carbamate was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06884821B1 |
| 出典データセット | uspto-grants-2005_04 |
| ORD ID | ord-2a1a9a721a2944d49cd57c440706ca11 |
| 出典メモ | uspto-grants-2005_04 |