Sodium → 1-[4-(3-Amino-1,2,4-oxadiazol-5-yl)phenyl]ethylamine

HRID 1729191

반응식

HRID 1729191 반응식
[Na].[OH:2][NH:3][C:4]([NH2:6])=[NH:5].[C:7]([C:10]1[CH:15]=[CH:14][C:13]([CH:16]([NH2:18])[CH3:17])=[CH:12][CH:11]=1)(O)=O>C(O)C>[NH2:5][C:4]1[N:6]=[C:7]([C:10]2[CH:15]=[CH:14][C:13]([CH:16]([NH2:18])[CH3:17])=[CH:12][CH:11]=2)[O:2][N:3]=1

참가 물질

5

반응물 3

HCID 5360545SodiumHCID 125682714-(1-Aminoethyl)benzoic acidHCID 178513189HCID 178513189, 화합물

생성물 1

HCID 199334461-[4-(3-Amino-1,2,4-oxadiazol-5-yl)phenyl]ethylamine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

0.8 g of sodium is dissolved in 60 ml of absolute ethanol, and 12 g of molecular sieve (4Å) and 2.63 g of N-hydroxyguanidine are added. The batch is stirred for 1 hour at room temperature and then 1.14 g of 1-(4-carboxyphenyl)ethylamine are added. The resulting turbid yellowish solution is heated under reflux for 2 hours after which time it can be established by thin layer chromatography that the reaction is complete. The batch is filtered and the solvent is removed under reduced pressure. The residue is digested in water and cooled in an ice bath, and then the precipitate is isolated by filtration, washed with a small amount of water and dried under reduced pressure to give 1-[4-(3-amino-1,2,4-oxadiazol-5-yl)phenyl]ethylamine having a melting point of 150°-151°.

후처리

  1. temperatureThe resulting turbid yellowish solution is heated
  2. temperatureunder reflux for 2 hours after which time it
  3. filtrationThe batch is filtered
  4. customthe solvent is removed under reduced pressure
  5. temperaturecooled in an ice bath
  6. customthe precipitate is isolated by filtration
  7. washwashed with a small amount of water
  8. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-e04455e8649d43bea3fe0a3657a88c87
출처 데이터셋
uspto-grants-1994_07
특허 번호
US05332729

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