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HRID 1081839作成日:2026年10月25日

Dimethyl Sulfate → 1H-Purine-2,6-dione, 3,7-dihydro-8-(2-(1,1'-biphenyl)-4-ylethenyl)-1,3-diethyl-7-methyl-, (E)-

https://huagongshe.com/reaction/1081839

反応式

関与物質

役割名称HCID仕込み量
反応物Dimethyl SulfateHCID 6497—
反応物Sodium HydroxideHCID 14798—
反応物1H-Purine-2,6-dione, 3,7-dihydro-8-(2-(1,1'-biphenyl)-4-ylethenyl)-1,3-diethyl-, (E)-HCID 6448939—
溶媒MethanolHCID 887—
溶媒WaterHCID 962—
生成物1H-Purine-2,6-dione, 3,7-dihydro-8-(2-(1,1'-biphenyl)-4-ylethenyl)-1,3-diethyl-7-methyl-, (E)-HCID 644894030.8%

反応手順

Compound 163 (1.50 g, 3.89 mmol) obtained in Reference Example 104 was suspended in a mixed solvent of 13 ml of water, 3.9 ml of a 2N aqueous solution of sodium hydroxide, and 7 ml of methanol. To the suspension was dropwise added 0.55 ml (5.83 mmol) of dimethyl sulfate, and the resultant mixture was stirred at 60° C. for 4 hours. Water (10 ml) was added thereto, and the deposited crystals were collected by filtration and dried. The obtained crude crystals were purified by silica gel column chromatography, followed by recrystallization from ethyl acetate to give 480 mg (yield 28%) of Compound 164 as yellow columns.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05587378
出典データセットuspto-grants-1996_12
ORD IDord-671f35c06e53455f928e3a5ec289d8b4
出典メモuspto-grants-1996_12