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

HRID 601621ノート

反応式

HRID 601621 の反応式
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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-85fabe98a36d485ab1df99a083387309
出典データセット
uspto-grants-2011_03
特許番号
US07902375B2

反応ノート

読み込み中…