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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
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Chloroethyl methyl sulfide | HCID 10965 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Lithium Bromide | HCID 82050 | — |
| 反応物 | 3-methyl-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione | HCID 10241423 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-methyl-6-(2-methylsulfanylethyl)-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione | HCID 19423333 | 45% |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05556854 |
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| 出典データセット | uspto-grants-1996_09 |
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| ORD ID | ord-82a2371955da43e1b96b6c197c37a35c |
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| 出典メモ | uspto-grants-1996_09 |
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