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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 | — |
| 触媒 | Triphenylphosphine | HCID 11776 | — |
| 触媒 | HCID 178418476 | HCID 178418476 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | HCID 178418416 | HCID 178418416 | — |
| 生成物 | Tert-butyl (5-formyl-2-methoxybenzyl)carbamate | HCID 22493931 | 75.1% |
反応手順
1.015 g of t-butyl N-(5-bromo-2-methoxybenzyl)carbamate, 45 mg of dichlorobis(triphenylphosphine)palladium (II), 330 mg of sodium formate and 17 mg of triphenylphosphine were dissolved in anhydrous N,N-dimethylformamide, followed by stirring for 2 hours at 110° C. in carbon monoxide atmosphere. The reaction mixture was diluted with ethyl acetate, and washed with water and saturated sodium bicarbonate water. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated. The residue was purified by silica gel column chromatography, and 640 mg of t-butyl N-(5-formyl-2-methoxybenzyl)carbamate was obtained from fractions eluted with hexane-ethyl acetate (3:1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07244861B2 |
| 出典データセット | uspto-grants-2007_07 |
| ORD ID | ord-04a0c5bca7cd4ea2a1e72ff93846ae5a |
| 出典メモ | uspto-grants-2007_07 |