Morpholine → 4-(N-t-butoxycarbonyl-N-methyl-beta-alanyl)morpholine

HRID 1649893ノート

反応式

HRID 1649893 の反応式
[C:1]([O:5][C:6]([N:8]([CH3:15])[CH:9](C)[CH2:10][C:11]([OH:13])=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].[NH:16]1[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1.Cl.C(N=C=NCCCN(C)C)C>C(Cl)Cl>[C:1]([O:5][C:6]([N:8]([CH3:15])[CH2:9][CH2:10][C:11]([N:16]1[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1)=[O:13])=[O:7])([CH3:2])([CH3:3])[CH3:4]

参加物

5

反応物 3

HCID 8083MorpholineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 190973273-{[(Tert-butoxy)carbonyl](methyl)amino}butanoic acid

生成物 1

HCID 197537714-(N-t-butoxycarbonyl-N-methyl-beta-alanyl)morpholine収率 106.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a mixture of N-t-butoxycarbonyl-N-methyl-β-methyl-β-alanine (1.02 g) and morpholine (0.48 g) in dry methylene chloride was added N-ethyl-N'-(3-dimethylaminopropyl)carbodiimide hydrochloride (1.05 g), and the mixture was stirred at ambient temperature overnight. After evaporation of the solvent, the residue was dissolved in ethyl acetate. The solution was washed with 1% citric acid aqueous solution, saturated sodium bicarbonate solution, and saturated sodium chloride solution. Then the solution was dried over magnesium sulfate and concentrated under reduced pressure to give 4-(N-t-butoxycarbonyl-N-methyl-β-alanyl)morpholine (1.36 g).

後処理

  1. customAfter evaporation of the solvent
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washThe solution was washed with 1% citric acid aqueous solution, saturated sodium bicarbonate solution, and saturated sodium chloride solution
  4. dry with materialThen the solution was dried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-d88a923aada649abaaad15c41faf4f9a
出典データセット
uspto-grants-1990_05
特許番号
US04921855

反応ノート

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