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Sodium hydride → (R)-1-(5-Acetoxyhexyl)-3-(2-furylmethyl)-7-pivaloyloxymethyl-8-methylxanthine

HRID 1421240
ノート
印刷プレビュー

反応式

HRID 1421240 の反応式
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][N:7]1[C:15]2[N:14]=[C:13]([CH3:16])[N:12]([CH2:17][O:18][C:19](=[O:24])[C:20]([CH3:23])([CH3:22])[CH3:21])[C:11]=2[C:10](=[O:25])[NH:9][C:8]1=[O:26].[H-].[Na+].[C:29]([O:32][C@H:33]([CH3:39])[CH2:34][CH2:35][CH2:36][CH2:37]I)(=[O:31])[CH3:30]>CS(C)=O>[C:29]([O:32][C@H:33]([CH3:39])[CH2:34][CH2:35][CH2:36][CH2:37][N:9]1[C:10](=[O:25])[C:11]2[N:12]([CH2:17][O:18][C:19](=[O:24])[C:20]([CH3:22])([CH3:23])[CH3:21])[C:13]([CH3:16])=[N:14][C:15]=2[N:7]([CH2:6][C:2]2[O:1][CH:5]=[CH:4][CH:3]=2)[C:8]1=[O:26])(=[O:31])[CH3:30]
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 24758Sodium hydrideHCID 187805583-(2-Furylmethyl)-7-pivaloyloxymethyl-8-methylxanthineHCID 54009360(R)-5-acetoxy-1-iodohexane

生成物 1

HCID 15481613(R)-1-(5-Acetoxyhexyl)-3-(2-furylmethyl)-7-pivaloyloxymethyl-8-methylxanthine収率 45.3%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

To a stirring solution of 3-(2-Furylmethyl)-7-pivaloyloxymethyl-8-methylxanthine (0.65 g, 1.8 mmol) in dimethyl sulfoxide (20 ml) was added sodium hydride in one portion. After 30 minutes, (R)-5-acetoxy-1-iodohexane (0.58 g, 2.16 mmol, prepared as above) was added neat. The reaction was allowed to stir at ambient temperature for 20 hours, quenched with water (70 ml) and then extracted with ethyl acetate (3×35 ml). The extracts were washed with saturated aqueous sodium chloride solution (30 ml), dried over sodium sulfate and concentrated to give a crude yellow oil. The product was purified by flash chromatography on silica gel (ethyl acetate) to give (R)-1-(5-Acetoxyhexyl)-3-(2-furylmethyl)-7-pivaloyloxymethyl-8-methylxanthine (0.41 g) as a yellow oil. The product oil was dissolved in methanol (20 ml) and treated with a sodium methoxide solution (25 wt. % in MeOH, 0.94 ml, 4.1 mmol). The reaction was allowed to stir at ambient temperature for 48 hours. The solution was diluted with ethyl acetate (40 ml) and quenched with water (20 ml). The organic phase was collected and washed with saturated aqueous sodium chloride solution (20 ml), dried over sodium sulfate and concentrated to give a yellow solid. Column chromatography on silica gel eluting with 10% methanol-ethyl acetate gave (R)-3-(2furylmethyl)-1-(5-hydroxyhexyl)-8-methylxanthin CT2412R (21 mg) as an off-white solid.

後処理

  1. customquenched with water (70 ml)
  2. extractionextracted with ethyl acetate (3×35 ml)
  3. washThe extracts were washed with saturated aqueous sodium chloride solution (30 ml)
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. customto give a crude yellow oil
  7. customThe product was purified by flash chromatography on silica gel (ethyl acetate)

出典と根拠

ORDレコード
ord-72c14694a4c84464bf84aa5752c5736e
出典データセット
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06075029

反応ノート

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