Hydrochloric Acid → (S)-1-(5-hydroxyhexyl)-7-benzyl-3-methylxanthine

HRID 1835735ノート

反応式

HRID 1835735 の反応式
C([O:4][C@@H:5]([CH3:29])[CH2:6][CH2:7][CH2:8][CH2:9][N:10]1[C:19](=[O:20])[C:18]2[N:17]([CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH:16]=[N:15][C:14]=2[N:13]([CH3:28])[C:11]1=[O:12])(=O)C.Cl>CO.CCOCC>[OH:4][C@@H:5]([CH3:29])[CH2:6][CH2:7][CH2:8][CH2:9][N:10]1[C:19](=[O:20])[C:18]2[N:17]([CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH:16]=[N:15][C:14]=2[N:13]([CH3:28])[C:11]1=[O:12]

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 53701359(S)-1-(5-acetoxyhexyl)-7-benzyl-3-methylxanthine

生成物 1

HCID 11610099(S)-1-(5-hydroxyhexyl)-7-benzyl-3-methylxanthine収率 86.2%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 3283Diethyl Ether溶媒

実験手順

A solution of (S)-1-(5-acetoxyhexyl)-7-benzyl-3-methylxanthine (350 mg) in methanol (10 ml) was treated with 1 M hydrogen chloride in ether (5 ml). After stirring at room temperature for 12 hours, the solvent was evaporated under reduced pressure. The residue was dissolved in dichloromethane (100 ml). The solution was washed with saturated aqueous sodium bicarbonate solution (30 ml), dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give (S)-1-(5-hydroxyhexyl)-7-benzyl-3-methylxanthine (270 mg).

後処理

  1. customthe solvent was evaporated under reduced pressure
  2. dissolutionThe residue was dissolved in dichloromethane (100 ml)
  3. washThe solution was washed with saturated aqueous sodium bicarbonate solution (30 ml)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-3d576104ca0d4f7c80dd80563d5514eb
出典データセット
uspto-grants-2004_08
特許番号
US06774130B2

反応ノート

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