Sodium → HCID 20535721, 화합물

HRID 1414012노트

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HRID 1414012 반응식
[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

참가 물질

5

반응물 3

HCID 5360545SodiumHCID 205357162-[4-(2-hydroxyethoxy)phenyl]acetonitrileHCID 20535719HCID 20535719, 화합물

생성물 1

HCID 20535721HCID 20535721, 화합물

시약·촉매·용매 1

HCID 8076Glycol monoethyl ether용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-441d9ff264c9496a97fa6c8eb827aefb
출처 데이터셋
uspto-grants-1981_02
특허 번호
US04252809

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