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HRID 1598797作成日:2026年10月26日

Dimethylformamide → 167356-39-0

https://huagongshe.com/reaction/1598797

反応式

関与物質

役割名称HCID仕込み量
反応物DimethylformamideHCID 6228—
反応物Sodium BicarbonateHCID 516892—
反応物Chloromethyl butanoateHCID 2725008—
反応物(4R)-1,4-dihydro-2,6-dimethyl-4-(2',3'-dichorophenyl)-5-carboxymethyl-3-pyridinecarboxylic acidHCID 22884797—
生成物167356-39-0HCID 2288479970%

反応条件

温度80 °C

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 chloromethylbutyrate (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% ethylacetate 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 for Compound C. [α]D20 =+17.5° (1% in methanol).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05739152
出典データセットuspto-grants-1998_04
ORD IDord-a3eae94728c54d09bd4956665ef4cd04
出典メモuspto-grants-1998_04