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tert-Butanol → 2-Nitro-terephthalic acid 1-tert-butyl ester 4-methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | tert-Butanol | HCID 6386 | — |
| 反応物 | Di-tert-butyl dicarbonate | HCID 90495 | — |
| 反応物 | 4-(Methoxycarbonyl)-2-nitrobenzoic acid | HCID 21906474 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Nitro-terephthalic acid 1-tert-butyl ester 4-methyl ester | HCID 67512782 | — |
反応手順
Commercially available 2-nitro-terephthalic acid 4-methyl ester (4.84 g, 21.49 mmol) in DCM (54 mL) was treated with tert-butanol (4.05 mL, 42.99 mmol), di-tert-butyl dicarbonate (12.19 g, 55.87 g) and DMAP (0.79 g, 6.45 mmol). After 4 days at room temperature, the reaction was diluted with DCM (100 mL), washed with 1N HCl (100 mL), aqueous NaHCO3 and finally with water. After drying over sodium sulphate and evaporation of the volatiles, the title compound was obtained as a brownish oil in more than quantitative yield (6.51 g). The crude was employed in the following step with no further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09102662B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-e1d2a6cc8b48444498af800db6310524 |
| 出典メモ | uspto-grants-2015_08 |