Benzylamine → HCID 86753041, compound

Participants

Reaction Steps

The compound obtained in Example 61 (0.50 g), 1 ml of DMF and 0.15 g of thionyl chloride were suspended in 10 ml of dichloromethane and refluxed for 3 hours. After completion of the reaction, the reaction mixture was allowed to cool, 10 ml of dichloromethane containing 0.14 g of benzylamine and 0.58 g of DBU was added dropwise, and the mixture was stirred at room temperature for 18 hours. After the reaction, the organic layer was washed with diluted hydrochloric acid, distilled water and saturated brine in this order, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue thus obtained was purified by silica gel column chromatography (eluent: dichloromethane: methanol=30:1) and recrystallized from ethyl acetate-n-hexane to provide 0.28 g of the desired compound as colorless crystals. Table 3 shows the chemical structure and physical property (melting point) of the compound obtained.

Provenance & Evidence