2,4-Dimethoxybenzonitrile → 1H-Purine, 8-(2,4-dimethoxyphenyl)-

HRID 1155063

反応式

HRID 1155063 の反応式
[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][N:5]=[CH:4][N:3]=1.[CH3:9][O:10][C:11]1[CH:18]=[C:17]([O:19][CH3:20])[CH:16]=[CH:15][C:12]=1[C:13]#N.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1C=CC=CC=1>[CH3:9][O:10][C:11]1[CH:18]=[C:17]([O:19][CH3:20])[CH:16]=[CH:15][C:12]=1[C:13]1[NH:8][C:7]2[C:2](=[N:3][CH:4]=[N:5][CH:6]=2)[N:1]=1

参加物

5

反応物 3

HCID 777502,4-DimethoxybenzonitrileHCID 837034,5-DiaminopyrimidineHCID 521998p-Toluenesulfonic acid monohydrate

生成物 1

HCID 30599121H-Purine, 8-(2,4-dimethoxyphenyl)-

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

反応条件

温度
120 °C

実験手順

A mixture of 2 g of 4,5-diamino-pyrimidine, 4 g of 2,4-dimethoxy-benzonitrile, 6 g of p-toluene sulfonic acid hydrate, and 40 ml of benzene was heated, whereby the benzene was distilled off. The residue was heated for 30 minutes at 120° C. After cooling the residue was triturated with 2 N ammonia and extracted with ethyl acetate. The ethyl acetate phase was extracted with 2 N hydrochloric acid, the aqueous phase was neutralized and again extracted with ethyl acetate, and subsequently the organic phase was extracted with 2 N sodium hydroxide solution. When the aqueous phase was neutralized, the product was precipitated and recrystallized from water.

後処理

  1. temperaturewas heated
  2. distillationwhereby the benzene was distilled off
  3. temperatureAfter cooling the residue
  4. customwas triturated with 2 N ammonia
  5. extractionextracted with ethyl acetate
  6. extractionThe ethyl acetate phase was extracted with 2 N hydrochloric acid
  7. extractionagain extracted with ethyl acetate
  8. extractionsubsequently the organic phase was extracted with 2 N sodium hydroxide solution
  9. customthe product was precipitated
  10. customrecrystallized from water

出典と根拠

ORDレコード
ord-63f0d60977ab4bd0987398e8ee4f424a
出典データセット
uspto-grants-1981_11
特許番号
US04299834

関連ノート

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