反応式
[CH3:1][N:2]1[C:7](=[O:8])[C:6]2[CH2:9][NH:10][CH2:11][CH2:12][C:5]=2[NH:4][C:3]1=[O:13].Cl[CH2:15][CH2:16][S:17][CH3:18].[Br-].[Li+].C(N(C(C)C)C(C)C)C>CN(C)C=O>[CH3:1][N:2]1[C:7](=[O:8])[C:6]2[CH2:9][N:10]([CH2:15][CH2:16][S:17][CH3:18])[CH2:11][CH2:12][C:5]=2[NH:4][C:3]1=[O:13]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
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.
後処理
- concentrationAfter the reaction mixture had been concentrated under reduced pressure
- extractionthe mixture was worked up by extraction with dichloromethane and water
出典と根拠
- ORDレコード
- ord-82a2371955da43e1b96b6c197c37a35c
- 出典データセット
- uspto-grants-1996_09
- 特許番号
- US05556854
関連ノート
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