Monoperoxyphthalic Acid Magnesium Salt → 3-Methyl-6-(2-methylsulfinylethyl)-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione

HRID 742970ノート

反応式

HRID 742970 の反応式
C(O[O-])(=O)C1C(=CC=CC=1)C([O-])=[O:5].[Mg+2].[CH3:15][N:16]1[C:21](=[O:22])[C:20]2[CH2:23][N:24]([CH2:27][CH2:28][S:29][CH3:30])[CH2:25][CH2:26][C:19]=2[NH:18][C:17]1=[O:31]>C(O)C>[CH3:15][N:16]1[C:21](=[O:22])[C:20]2[CH2:23][N:24]([CH2:27][CH2:28][S:29]([CH3:30])=[O:5])[CH2:25][CH2:26][C:19]=2[NH:18][C:17]1=[O:31]

参加物

4

反応物 2

HCID 10130449Monoperoxyphthalic Acid Magnesium SaltHCID 194233333-methyl-6-(2-methylsulfanylethyl)-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione

生成物 1

HCID 194233603-Methyl-6-(2-methylsulfinylethyl)-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
55 °C

実験手順

21.8 g of magnesium monoperoxyphthalate (85% pure) were added at 55° C. over a period of 15 min to a solution of 19.5 g of 3-methyl-6-(2-methylsulfanylethyl)-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione in 200 ml of ethanol and the mixture was stirred for 2 h at 55° C. After the pH had been adjusted to 7.5, the mixture was concentrated under reduced pressure. The residue was boiled up several times with methanol, the combined methanol phases were concentrated and the residue was purified by chromatography in a medium-pressure column with silica gel using dichloromethane/methanol (volume ratio 95:5) as the eluent and by recrystallization from isopropanol.

後処理

  1. concentrationthe mixture was concentrated under reduced pressure
  2. concentrationthe combined methanol phases were concentrated
  3. customthe residue was purified by chromatography in a medium-pressure column with silica gel
  4. customby recrystallization from isopropanol

出典と根拠

ORDレコード
ord-f5c4cc555ad7444194912a8cd30088a2
出典データセット
uspto-grants-1996_09
特許番号
US05556854

反応ノート

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