Kfm 19 → 1,3-Dipropyl-8-(1-hydroxycyclopent-3-yl)xanthine

HRID 1734179노트

반응식

HRID 1734179 반응식
[CH2:1]([N:4]1[C:13](=[O:14])[C:12]2[NH:11][C:10]([CH:15]3[CH2:19][CH2:18][C:17](=[O:20])[CH2:16]3)=[N:9][C:8]=2[N:7]([CH2:21][CH2:22][CH3:23])[C:5]1=[O:6])[CH2:2][CH3:3]>C(O)C>[CH2:1]([N:4]1[C:13](=[O:14])[C:12]2[NH:11][C:10]([CH:15]3[CH2:19][CH2:18][CH:17]([OH:20])[CH2:16]3)=[N:9][C:8]=2[N:7]([CH2:21][CH2:22][CH3:23])[C:5]1=[O:6])[CH2:2][CH3:3]

참가 물질

3

반응물 1

HCID 131584Kfm 19

생성물 1

HCID 103813391,3-Dipropyl-8-(1-hydroxycyclopent-3-yl)xanthine수율 78%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

0.5 g (1.6 mmol) of 1,3-dipropyl-8-(1-oxo-3-cyclopentyl)xanthine, 10 ml of ethanol and 0.1 g (2.6 mmol) of sodium tetrahydridoboranate are stirred for 21/2 days at ambient temperature. The mixture is evaporated down in vacuo and mixed with water and methylene chloride then the aqueous phase is acidified and extracted. The combined organic extracts are dried and evaporated down in vacuo. The residue is separated into the isomers by chromatography on silica gel (CH2Cl2 /CH3OH 95:5). From the 1st fraction, 0.4 g of the title compound are obtained in the form of white crystals (39% of theory), m.p. 174°-176° C. and from the 2nd fraction 0.4 g of the title compound are obtained in the form of white crystals (39% of theory), m.p. 191°-193° C.

후처리

  1. customThe mixture is evaporated down in vacuo
  2. additionmixed with water and methylene chloride
  3. extractionextracted
  4. customThe combined organic extracts are dried
  5. customevaporated down in vacuo
  6. customThe residue is separated into the isomers by chromatography on silica gel (CH2Cl2 /CH3OH 95:5)

출처 및 근거

ORD 기록
ord-16e7fcdd7f9542baab0179e5537f11f5
출처 데이터셋
uspto-grants-1996_07
특허 번호
US05532368

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