Sodium → HCID 20535721、化合物

HRID 1414012ノート

反応式

HRID 1414012 の反応式
[Na].[NH2:2][C:3]1[N:8]=[C:7]([N:9]=O)[N:6]=[C:5]([NH2:11])[C:4]=1[NH2:12].[OH:13][CH2:14][CH2:15][O:16][C:17]1[CH:22]=[CH:21][C:20]([CH2:23][C:24]#[N:25])=[CH:19][CH:18]=1>C(OCCO)C>[NH2:9][C:7]1[N:6]=[C:5]([NH2:11])[C:4]2[C:3](=[N:2][C:24]([NH2:25])=[C:23]([C:20]3[CH:19]=[CH:18][C:17]([O:16][CH2:15][CH2:14][OH:13])=[CH:22][CH:21]=3)[N:12]=2)[N:8]=1

参加物

5

反応物 3

HCID 5360545SodiumHCID 205357162-[4-(2-hydroxyethoxy)phenyl]acetonitrileHCID 20535719HCID 20535719、化合物

生成物 1

HCID 20535721HCID 20535721、化合物

試薬・触媒・溶媒 1

HCID 8076Glycol monoethyl ether溶媒

実験手順

460 mg of metallic sodium are dissolved with stirring in 150 ml of 2-ethoxy-ethanol. 3.1 g (0.02 mol) of triaminonitroso-pyrimidine and 3.5 g (0.02 mol) of p-(2-hydroxyethoxy)phenyl-acetonitrile are added one after the other with stirring and the mixture is heated with stirring in a water bath at 60° C. The color of the mixture changes from violet to bright brown. After stirring for 14 hours, the reaction is over. The mixture is left to cool. Unreacted 2,4,6-triamino-nitrosopyrimidine is filtered off and the clear solution is concentrated to dryness. The precipitate is taken up in hot acetone and the crude product is precipitated by admixture with petroleum ether. Purification follows first by recrystallization from butanol and then by separation on a silica gel-dry column (silica gel 60 Merck). The compound mentioned in the title is obtained as yellow-brown crystals.

後処理

  1. temperaturethe mixture is heated
  2. stirringwith stirring in a water bath at 60° C
  3. stirringAfter stirring for 14 hours
  4. waitThe mixture is left
  5. temperatureto cool
  6. filtrationUnreacted 2,4,6-triamino-nitrosopyrimidine is filtered off
  7. concentrationthe clear solution is concentrated to dryness
  8. customthe crude product is precipitated by admixture with petroleum ether
  9. customPurification
  10. customfollows first by recrystallization from butanol
  11. customby separation on a silica gel-
  12. customdry column (silica gel 60 Merck)
  13. customis obtained as yellow-brown crystals

出典と根拠

ORDレコード
ord-441d9ff264c9496a97fa6c8eb827aefb
出典データセット
uspto-grants-1981_02
特許番号
US04252809

反応ノート

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