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Hydrochloric Acid → 6-(4-Hydroxybutyl)-3-methyl-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione

HRID 742972
ノート
印刷プレビュー

反応式

HRID 742972 の反応式
[CH3:1][N:2]1[C:7](=[O:8])[C:6]2[CH2:9][N:10]([CH2:13][CH2:14][CH2:15][CH2:16][O:17]C3CCCCO3)[CH2:11][CH2:12][C:5]=2[NH:4][C:3]1=[O:24].O.Cl>CO>[OH:17][CH2:16][CH2:15][CH2:14][CH2:13][N:10]1[CH2:11][CH2:12][C:5]2[NH:4][C:3](=[O:24])[N:2]([CH3:1])[C:7](=[O:8])[C:6]=2[CH2:9]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 194233293-methyl-6-[4-(tetrahydropyran-2-yloxy)butyl]-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione

生成物 1

HCID 194233386-(4-Hydroxybutyl)-3-methyl-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

12 g of 3-methyl-6-[4-(tetrahydropyran-2-yloxy)butyl]-5,6,7,8-tetrahydro-1H-pyrido[4,3-d]pyrimidine-2,4-dione were dissolved in 150 ml of methanol and 150 ml of water and the pH was adjusted to i with conc. hydrochloric acid at 20°-25° C., with stirring. After 7 h at room temperature, the mixture was concentrated to dryness under reduced pressure, the residue was taken up with water and the solution was adjusted to pH 7.8. It was concentrated under vacuum and the residue was extracted exhaustively with hot ethanol. The ethanolic extract was evaporated under reduced pressure and the crude 6-(4-hydroxybutyl)-3-methyl-5,6,7,8-tetrahydro-1H-pyrido-[4,3-d]pyrimidine-2,4-dione was purified by column chromatography on silica gel with dichloromethane/methanol (volume ratio 90:10) and by recrystallization from isopropanol.

後処理

  1. concentrationthe mixture was concentrated to dryness under reduced pressure
  2. concentrationIt was concentrated under vacuum
  3. extractionthe residue was extracted exhaustively with hot ethanol
  4. extractionThe ethanolic extract
  5. customwas evaporated under reduced pressure
  6. customthe crude 6-(4-hydroxybutyl)-3-methyl-5,6,7,8-tetrahydro-1H-pyrido-[4,3-d]pyrimidine-2,4-dione was purified by column chromatography on silica gel with dichloromethane/methanol (volume ratio 90:10) and by recrystallization from isopropanol

出典と根拠

ORDレコード
ord-48683d181c36403fa8e52779b6e02e28
出典データセット
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05556854

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート