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Sulfuric Acid → HCID 20392968、化合物

HRID 1863131
ノート
印刷プレビュー

反応式

HRID 1863131 の反応式
[C:1]([C:3]1[CH:4]=[CH:5][C:6]([O:19][CH2:20][CH2:21][CH3:22])=[C:7]([C:9]2[N:17]=[C:16]3[C:12](=[N:13][N:14]=[N:15]3)[C:11](=[O:18])[N:10]=2)[CH:8]=1)#[N:2].S(=O)(=O)(O)[OH:24]>O>[C:1]([C:3]1[CH:4]=[CH:5][C:6]([O:19][CH2:20][CH2:21][CH3:22])=[C:7]([C:9]2[N:17]=[C:16]3[C:12](=[N:13][N:14]=[N:15]3)[C:11](=[O:18])[N:10]=2)[CH:8]=1)(=[O:24])[NH2:2]
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 1118Sulfuric AcidHCID 20392959HCID 20392959、化合物

生成物 1

HCID 20392968HCID 20392968、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

2-(5-Cyano-2-propoxyphenyl)-8-azapurin-6-one (2.0 g; prepared as described in Example 6) was carefully added with stirring to concentrated sulphuric acid (20 ml) during 10 minutes. The resulting solution was allowed to stand at room temperature for 3 hours, and then it was poured into iced water (100 ml) and the mixture was allowed to stand for 2 hours. The resulting solid was then filtered off and dissolved in aqueous sodium carbonate solution (2 N; 50 ml). This solution was treated with charcoal, filtered, and acidified by the addition of concentrated hydrochloric acid, and the resulting white solid was recrystallised from dimethylformamide. The recrystallised solid was dissolved in aqueous sodium carbonate solution (2 N; 50 ml) and the solution was acidified by the addition of concentrated hydrochloric acid and the resulting solid was filtered off to give 2-(5-carbamoyl-2-propoxyphenyl)-8-azapurin-6-one (0.9 g), m.p. 273°-275° C. (with decomposition).

後処理

  1. waitto stand for 2 hours
  2. filtrationThe resulting solid was then filtered off
  3. dissolutiondissolved in aqueous sodium carbonate solution (2 N; 50 ml)
  4. additionThis solution was treated with charcoal
  5. filtrationfiltered
  6. additionacidified by the addition of concentrated hydrochloric acid
  7. customthe resulting white solid was recrystallised from dimethylformamide
  8. dissolutionThe recrystallised solid was dissolved in aqueous sodium carbonate solution (2 N; 50 ml)
  9. additionthe solution was acidified by the addition of concentrated hydrochloric acid
  10. filtrationthe resulting solid was filtered off

出典と根拠

ORDレコード
ord-c8c353178c6849a8989fad02cc9b96ae
出典データセット
uspto-grants-1979_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04167568

反応ノート

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