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Benzoic Acid → 3,9-Dihydro-8-phenyl-1,3-dipropyl-1H-purine-2,6-dione

HRID 1981584
ノート
印刷プレビュー

反応式

HRID 1981584 の反応式
[CH2:1]([N:4]1[C:11]([NH2:12])=[C:10]([NH2:13])[C:8](=[O:9])[N:7]([CH2:14][CH2:15][CH3:16])[C:5]1=[O:6])[CH2:2][CH3:3].[C:17](O)(=O)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>CO>[CH2:14]([N:7]1[C:8](=[O:9])[C:10]2[NH:13][C:17]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[N:12][C:11]=2[N:4]([CH2:1][CH2:2][CH3:3])[C:5]1=[O:6])[CH2:15][CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 243Benzoic AcidHCID 50986055,6-Diamino-1,3-dipropyl-2,4(1H,3H)-pyrimidinedione

生成物 1

HCID 1287843,9-Dihydro-8-phenyl-1,3-dipropyl-1H-purine-2,6-dione収率 77%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

1,3-dipropyl-5,6-diaminouracil (0.01 mol) was dissolved in 30 ml methanol, followed by 0.01 mol of benzoic acid and then 0.01 mol of DICD. The solution was stirred for 30 min at room temperature, filtered, and washed with a small amount of methanol. The solid was boiled for ten minutes in 2.5N KOH, filtered hot, and the liquid neutralized with concentrated HCl. The solid was collected by filtration, washed with water, redissolved in 100 ml with a minimum amount of KOH, precipitated by neutralization with HCL, filtered, washed with water, and dried. The product was identified by chemical ionization mass spectrometry and elemental analysis. Yield 77%.

後処理

  1. filtrationfiltered
  2. washwashed with a small amount of methanol
  3. waitThe solid was boiled for ten minutes in 2.5N KOH
  4. filtrationfiltered hot
  5. filtrationThe solid was collected by filtration
  6. washwashed with water
  7. dissolutionredissolved in 100 ml with a minimum amount of KOH
  8. customprecipitated by neutralization with HCL
  9. filtrationfiltered
  10. washwashed with water
  11. customdried

出典と根拠

ORDレコード
ord-0462b2d84e6240458c85d00454c61e8b
出典データセット
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04593095

反応ノート

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