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

HRID 742970노트

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HRID 742970 반응식
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]

참가 물질

4

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
55 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f5c4cc555ad7444194912a8cd30088a2
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05556854

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