Formate → 2-(5-Ethyloxazol-2-yl)ethylamine

HRID 601621노트

반응식

HRID 601621 반응식
C([O-])=O.C(OC(=O)[NH:13][CH2:14][CH2:15][C:16]1[O:17][C:18]([CH2:21][CH3:22])=[CH:19][N:20]=1)C1C=CC=CC=1>CO.[Pd]>[CH2:21]([C:18]1[O:17][C:16]([CH2:15][CH2:14][NH2:13])=[N:20][CH:19]=1)[CH3:22]

참가 물질

5

반응물 2

HCID 283FormateHCID 57636953Benzyl [2-(5-ethyloxazol-2-yl)ethyl]carbamate

생성물 1

HCID 115428012-(5-Ethyloxazol-2-yl)ethylamine

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

Ammnonium formate (0.316 g, 5 mmol) is added to a solution of [2-(5-ethyl-oxazol-2-yl)-ethyl]-carbamic acid benzyl ester (step 3) (1.66 mmol) in methanol (15 ml) and 10% Pd on carbon (125 mg) is added under an inert atmosphere. The mixture is stirred at ambient temperature for 2 hours. The catalyst is removed by filtration and the filtrate is evaporated. The residue is diluted with dichloromethane, filtered to remove undissolved solid and the solvent is removed. The residue is dissolved in DCM and treated with 1M aqueous sodium hydroxide solution (5 ml). The organic extract is separated, dried (MgSO4), filtered and the solvent is removed. Crystallisation from ethyl acetate/dichloromethane affords the titled compound.

후처리

  1. additionis added under an inert atmosphere
  2. customThe catalyst is removed by filtration
  3. customthe filtrate is evaporated
  4. additionThe residue is diluted with dichloromethane
  5. filtrationfiltered
  6. customto remove undissolved solid
  7. customthe solvent is removed
  8. dissolutionThe residue is dissolved in DCM
  9. additiontreated with 1M aqueous sodium hydroxide solution (5 ml)
  10. extractionThe organic extract
  11. customis separated
  12. dry with materialdried (MgSO4)
  13. filtrationfiltered
  14. customthe solvent is removed
  15. customCrystallisation from ethyl acetate/dichloromethane

출처 및 근거

ORD 기록
ord-85fabe98a36d485ab1df99a083387309
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07902375B2

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