関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Chloromethyl butanoate | HCID 2725008 | — |
| 反応物 | HCID 22884797 | HCID 22884797 | — |
| 生成物 | 167356-39-0 | HCID 22884799 | 70% |
反応手順
To a stirred mixture of (4R)-1,4-dihydro-2,6-dimethyl-4-(2',3'-dichorophenyl)-5-carboxymethyl-3-pyridinecarboxylic acid (2.93 g, 8.23 mmol) and sodium bicarbonate (1.38 g, 16.5 mmol) in DMF (150 ml) under nitrogen atmosphere was added chloromethyl butyrate (1.72 g, 12.6 mmol). The reaction mixture was heated at 80° C. for 17 h. Workup by filtration followed by evaporation of solvent. The crude residue was chromatographed on silica gel with 5% ethyl acetate in dichloromethane. Recrystallization from diisopropylether gave colorless crystals (2.62 g, 70%), mp. 128°-129° C. NMR spectral data are identical with the data of the racemate as shown in Example 3. [α]D20 =+17.5° (1% in methanol).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05856346 |
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| 出典データセット | uspto-grants-1999_01 |
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| ORD ID | ord-87aacaf89f584194a518128384d95ddc |
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| 出典メモ | uspto-grants-1999_01 |
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