関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Picolinic acid | HCID 1018 | — |
| 反応物 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 反応物 | 2,3-Dimethyliodobenzene | HCID 141645 | — |
| 反応物 | 2-(4-Hydroxy-phenyl)-morpholine-4-carboxylic acid tert-butyl ester | HCID 66654239 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | HCID 66653709 | HCID 66653709 | — |
反応手順
To a degassed solution of 2-(4-hydroxy-phenyl)-morpholine-4-carboxylic acid tert-butyl ester (10.23 g; 36.6 mmol), and 1-iodo-2,3-dimethyl-benzene (10.62 g; 45.8 mmol) in DMSO (50 mL), was added picolinic acid (0.90 g; 7.3 mmol), CuI (0.70 g; 3.7 mmol) and K3PO4 (15.55 g; 73.3 mmol). The resulting mixture was heated overnight, at 90° C. After cooling to RT, brine was added and the mixture extracted with CH2Cl2. The combined organic layers were dried (Na2SO4), filtered and concentrated in vacuo. The residue was purified by column chromatography (SiO2, CH2Cl2) to afford 2-[4-(2,3-dimethyl-phenoxy)-phenyl]-morpholine-4-carboxylic acid tert-butyl ester.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09029371B2 |
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| 出典データセット | uspto-grants-2015_05 |
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| ORD ID | ord-d646cfaf2d234009a22bae0a8e0e0f5d |
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| 出典メモ | uspto-grants-2015_05 |
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