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Under a nitrogen atmosphere, 0.8 g of methanesulfonyl chloride,Tetrahydrofuran 5 mL,10 mg of 2,6-di-tert-butyl-4-methylphenol was added.It was cooled to -5 ° C.,A solution prepared by dissolving 1.8 g of the compound represented by the formula (D-2 R-7) in 10 mL of tetrahydrofuran and 0.8 g of diisopropylethylamine were added dropwise, followed by stirring at -5 ° C. for 1 hour.8 mL of a tetrahydrofuran solution of 1.6 g of a compound represented by the formula (D-2 R-3), 0.8 g of diisopropylethylamine,10 mg of 4-dimethylaminopyridine was added,And the mixture was stirred at room temperature for 2 hours. The reaction solution was poured into water and extracted with dichloromethane. Purification by column chromatography (silica gel, dichloromethane) and recrystallization (dichloromethane / methanol) gave 2.3 g of a compound represented by the formula (D-2R). Purity 95.186percent
In a reaction vessel equipped with a Dean-Stark apparatus and a condenser, 10.0 g of the compound represented by the formula (C-4-1)15.2 g of the compound represented by the formula (C-4-2), 0.8 g of phosphoric acid,150 mL of mesitylene was added,And heated under reflux for 20 hours while removing water.After cooling, the solid was filtered and dispersed and washed with water. And dried to obtain 21.8 g of a compound represented by the formula (C-4). Under a nitrogen atmosphere,2.0 g of the compound represented by the formula (C-4) produced in Example 1-7,4.0 g of the compound represented by formula (D-2-1)0.1 g of 4-dimethylaminopyridine,40 mL of dichloromethane was added.2.1 g of diisopropylcarbodiimide was added dropwise while cooling with ice, and the mixture was stirred at room temperature for 10 hours.The precipitate was removed by filtration, and the filtrate was washed successively with 1percent hydrochloric acid, water and brine.After recrystallization (dichloromethane / methanol), purification was carried out by column chromatography (silica gel, dichloromethane) and recrystallization (dichloromethane / methanol) to obtain 4.6 g of the compound represented by the formula (D-2) .The obtained compound had a purity of 98.644percent (impurity content represented by formula (C-4) of 0.006percent, impurity content represented by formula (F1-2) and formula (F2-2) 0.120percent).
Under a nitrogen atmosphere,To the reaction vessel, 1.0 g of methanesulfonyl chloride,Tetrahydrofuran 5 mL,10 mg of 2,6-di-tert-butyl-4-methylphenol was added.It was cooled to -5 ° C.,A solution prepared by dissolving 2.0 g of the compound represented by the formula (D-2R-1) in 10 mL of tetrahydrofuran and 1.3 g of diisopropylethylamine were added dropwise, followed by stirring at -5 ° C. for 1 hour.4 mL of a tetrahydrofuran solution of 0.8 g of a compound represented by the formula (D-2 R-2), 1.3 g of diisopropylethylamine,10 mg of 4-dimethylaminopyridine was added, and the mixture was stirred at room temperature for 2 hours.The reaction solution was poured into 5percent hydrochloric acid and extracted with ethyl acetate.Purification by column chromatography (silica gel, ethyl acetate) gave 2.1 g of a compound represented by the formula (D-2 R-3).
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