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Water → Pyrazolo[3,4-d]pyrimidin-4-one

HRID 1597841
ノート
印刷プレビュー

反応式

HRID 1597841 の反応式
[Na].C1([N:7]2[C:11]([NH2:12])=[C:10]([C:13]([NH2:15])=[O:14])[C:9](CC)=[N:8]2)CCCC1.[CH2:18](OC1C=CC=CC=1C(OCC)=O)C=C.O>C(O)C.CCOCC>[N:7]1[C:11]2=[N:12][CH:18]=[N:15][C:13](=[O:14])[C:10]2=[CH:9][N:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 5360545SodiumHCID 10398065Benzoic acid, 2-(2-propenyloxy)-, ethyl esterHCID 224493525-amino-1-cyclopentyl-3-ethyl-1H-pyrazole-4-carboxamide

生成物 1

HCID 22252149Pyrazolo[3,4-d]pyrimidin-4-one

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回
HCID 3283
Diethyl Ether
溶媒

実験手順

Sodium spheres (207 mg) was dissolved in ethanol (15 ml) and 1-cyclopentyl-3-ethyl-5-amino-1H-pyrazole-4-carboxamide (1 g, 45 mmol) was added, followed by ethyl 2-(2-propenyloxy)benzoate (1.85 g, 9 mmol). The reaction mixture was refluxed overnight, cooled, the ethanol was stripped and water was added. The pH was adjusted to about 7 and a solid was isolated by filtration. The solid was taken up in ether, washed with dilute HCl, dried over MgSO4, filtered and the solvent was removed and the solid residue was recrystallized from ether to afford 0.56 g of 1-cyclopentyl-3-ethyl-6-[2-(CH2 =CH--CH2 O)phenyl]pyrazolo[3,4-d]pyrimidin-4-one, m.p. 119°-120° C.

後処理

  1. temperatureThe reaction mixture was refluxed overnight
  2. temperaturecooled
  3. customa solid was isolated by filtration
  4. washwashed with dilute HCl
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. customthe solvent was removed
  8. customthe solid residue was recrystallized from ether

出典と根拠

ORDレコード
ord-509372b60ff240d788cfd8a0a574b1ee
出典データセット
uspto-grants-1998_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05736548

反応ノート

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