Water → HCID 20535721、化合物

HRID 1156268ノート

反応式

HRID 1156268 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.O>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

6

反応物 4

HCID 962WaterHCID 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 metallic sodium were dissolved while stirring in 150 ml 2-ethoxyethanol. Thereafter to it was added while stirring 3.1 g (0.02 mole) of triamino-nitrosopyrimidine and 2.5 g (0.02 mole) p-(2-hydroxyethoxy)-phenyl acetonitrile and the mixture was stirred and heated in the water bath at 60° C. The color of the mixture changed from violet to light brown. After 14 hours of stirring, the reaction was stopped. The mixture is then allowed to cool. Unreacted 2,4,6-triamino-nitrosopyrimidine is filtered and the clear solution is evaporated and its volume reduced. The precipitate was taken up in hot acetone and by addition of petroleum ether, the raw product precipitated. The purification consisted of one recrystallization in butanol and also by passage through a silica gel column (Kieselgel 60, Merck). The title compound is obtained as yellowish-brown crystals.

後処理

  1. additionThereafter to it was added
  2. stirringAfter 14 hours of stirring
  3. temperatureto cool
  4. filtrationUnreacted 2,4,6-triamino-nitrosopyrimidine is filtered
  5. customthe clear solution is evaporated
  6. additionThe precipitate was taken up in hot acetone and by addition of petroleum ether
  7. customthe raw product precipitated
  8. customThe purification
  9. customconsisted of one recrystallization in butanol and also by passage through a silica gel column (Kieselgel 60, Merck)

出典と根拠

ORDレコード
ord-aaa331dd0428411fb786e6a3cea82604
出典データセット
uspto-grants-1982_06
特許番号
US04335119

反応ノート

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