Alloxan → 1,2,3,4-Tetrahydrobenzopteridine-2,4-dione

HRID 2413320ノート

反応式

HRID 2413320 の反応式
[C:1]1([NH2:8])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH2:7].[NH:9]1[C:17](=O)[C:15](=O)[C:13](=[O:14])[NH:12][C:10]1=[O:11]>O>[CH:4]1[CH:5]=[CH:6][C:1]2[C:2](=[N:7][C:15]3[C:13](=[O:14])[NH:12][C:10](=[O:11])[NH:9][C:17]=3[N:8]=2)[CH:3]=1

参加物

4

反応物 2

HCID 5781AlloxanHCID 7243O-Phenylenediamine

生成物 1

HCID 53727201,2,3,4-Tetrahydrobenzopteridine-2,4-dione

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

There was charged 800 ml of water into an Erlenmeyer flask, then 3.5 g (30 mmoles) of o-phenylenediamine and 5.0 g (30 mmoles) of alloxan were added thereto, and the mixture was stirred at room temperature in a nitrogen atmosphere for about 5 hours. The obtained reaction mixture was cooled with ice for 3 hours, then the formed yellow precipitate was filtered off, and washed in ethanol and ether (50 ml, twice). This precipitate was recrystallized from an aqueous dimethylformamide solution to give pale yellow powdery crystals. Yield: 7.5 g (90%). M.p. 300° C. or higher. IR spectrum: Found values (cm-1): 1730, 1705 (C=O stretching), 1572 (Broad peak) --C=N (amide II band). Literature values (cm-1): 1727, 1700, 1574.

後処理

  1. customThe obtained reaction mixture
  2. temperaturewas cooled with ice for 3 hours
  3. filtrationthe formed yellow precipitate was filtered off
  4. washwashed in ethanol
  5. customThis precipitate was recrystallized from an aqueous dimethylformamide solution
  6. customto give pale yellow powdery crystals

出典と根拠

ORDレコード
ord-97d95692c4944e929ff023ee775a4fa8
出典データセット
uspto-grants-1985_01
特許番号
US04496646

反応ノート

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