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HRID 742969作成日:2026年10月25日

2-Chloroethyl methyl sulfide → 3-methyl-6-(2-methylsulfanylethyl)-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione

https://huagongshe.com/reaction/742969

反応式

関与物質

役割名称HCID仕込み量
反応物2-Chloroethyl methyl sulfideHCID 10965—
反応物DiisopropylethylamineHCID 81531—
反応物Lithium BromideHCID 82050—
反応物3-methyl-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dioneHCID 10241423—
溶媒DimethylformamideHCID 6228—
生成物3-methyl-6-(2-methylsulfanylethyl)-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dioneHCID 1942333345%

反応手順

36.3 g of 3-methyl-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]-pyrimidine-2,4-dione, 23 g of 1-chloro-2-methylsulfanylethane (97% pure), 17.4 g of lithium bromide and 27 g of ethyldiisopropylamine in 700 ml of dimethylformamide were stirred for 14 h at 50° C. After the reaction mixture had been concentrated under reduced pressure, the residue was taken up with 400 ml of water and 400 ml, of dichloromethane, the pH was adjusted to 8 with sodium bicarbonate, with stirring, and the mixture was worked up by extraction with dichloromethane and water. 23 g of 3-methyl-6-(2-methylsulfanylethyl)-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione were obtained from the combined dichloromethane phases after drying, concentration and recrystallization of the residue from isopropanol.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05556854
出典データセットuspto-grants-1996_09
ORD IDord-82a2371955da43e1b96b6c197c37a35c
出典メモuspto-grants-1996_09