関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 2,4-Dihydroxybenzoic Acid | HCID 1491 | — |
| 反応物 | Isobutylene | HCID 8255 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2,4-Dihydroxy benzoic acid tert-butyl ester | HCID 21783547 | — |
反応手順
To a solution of 2,4-dihydroxy benzoic acid (3.08 g; 20 mmol) in dioxane (50 mL) was added conc. H2SO4 (3 mL) and the solution was cooled to −50° C. Isobutene (40 g) was added, the reaction flask sealed and allowed to warm to room temperature. The reaction mixture was stirred overnight, cooled to −30° C. and pH adjusted to 8 using saturated NaHCO3 (aq). The organic phase was Isolated, dried, evaporated to dryness and purified by column chromatography (SiO2-heptane/EtOAc=4:1) to yield 2.3 g (54%). MS (LC-MS): 209 (MH−).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07741352B2 |
|---|
| 出典データセット | uspto-grants-2010_06 |
|---|
| ORD ID | ord-4671f261620a43e7a6758dd6c1540ef9 |
|---|
| 出典メモ | uspto-grants-2010_06 |
|---|
