참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | Chloromethyl butanoate | HCID 2725008 | — |
| 반응물 | HCID 22884797 | HCID 22884797 | — |
| 생성물 | 167356-39-0 | HCID 22884799 | 70% |
반응 단계
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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05856346 |
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| 출처 데이터셋 | uspto-grants-1999_01 |
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| ORD ID | ord-87aacaf89f584194a518128384d95ddc |
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| 출처 메모 | uspto-grants-1999_01 |
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