(R)-1-(5-hydroxyhexyl)-7-benzyl-3,8-dimethylxanthine → (R)-1-(5-Hydroxyhexyl)-3,8-dimethylxanthine

HRID 1421234노트

반응식

HRID 1421234 반응식
C([N:8]1[C:16]2[C:15](=[O:17])[N:14]([CH2:18][CH2:19][CH2:20][CH2:21][C@H:22]([OH:24])[CH3:23])[C:13](=[O:25])[N:12]([CH3:26])[C:11]=2[N:10]=[C:9]1[CH3:27])C1C=CC=CC=1>C(O)(=O)C.C(OCC)(=O)C.[Pd]>[OH:24][C@H:22]([CH3:23])[CH2:21][CH2:20][CH2:19][CH2:18][N:14]1[C:15](=[O:17])[C:16]2[NH:8][C:9]([CH3:27])=[N:10][C:11]=2[N:12]([CH3:26])[C:13]1=[O:25]

참가 물질

5

반응물 1

HCID 9929299(R)-1-(5-hydroxyhexyl)-7-benzyl-3,8-dimethylxanthine

생성물 1

HCID 9860506(R)-1-(5-Hydroxyhexyl)-3,8-dimethylxanthine

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 176Acetic Acid용매HCID 8857Ethyl Acetate용매

실험 절차

A solution of (R)-7-benzyl-1-(5-hydroxyhexyl)-3,8-dimethylxanthine (250 mg) in a mixture of acetic acid (10 ml) and ethyl acetate (10 ml) was hydrogenated in presence of palladium on carbon (50 mg) for 12 hours. The mixture was filtered through celite (5 g) and concentrated. The residue was dissolved in ethyl acetate (100 ml), washed with saturated sodium bicarbonate solution (50 ml), dried over magnesium sulfate and concentrated. The product was purified by flash chromatography (silica gel) eluting with 10% methanol/ethyl acetate. Yield=180 mg.

후처리

  1. filtrationThe mixture was filtered through celite (5 g)
  2. concentrationconcentrated
  3. dissolutionThe residue was dissolved in ethyl acetate (100 ml)
  4. washwashed with saturated sodium bicarbonate solution (50 ml)
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated
  7. customThe product was purified by flash chromatography (silica gel)
  8. washeluting with 10% methanol/ethyl acetate

출처 및 근거

ORD 기록
ord-cdbf8b9e8e2549128cd734aeea957ba9
출처 데이터셋
uspto-grants-2000_06
특허 번호
US06075029

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