反応 #74417

ord-aa2b4b99706d4e52bae183b3613215c1

反応方程式

CCOC(=O)C(C)(O)C(C)C
ethyl 2-hydroxy-2,3-dimethylbutanoate
Cl.N=C(N)N
guanidine hydrochloride
O=C([O-])[O-].[K+].[K+]
K2CO3
CC(C)C1(C)OC(N)=NC1=O
product
CC(C)C1(C)OC(N)=NC1=O
2-Amino-5-isopropyl-5-methyl-1,3-oxazol-4(5H)-one

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度under reflux for 20 h
  2. 2
    その他The solvent was removed
  3. 3
    その他the residue was purified by silica gel flash chromatography (ethyl acetate/methanol 9:1)

実験手順

A mixture of ethyl 2-hydroxy-2,3-dimethylbutanoate (2.92 g, 18.2 mmol), guanidine hydrochloride (1.74 g, 18.2 mmol), and K2CO3 (2.52 g, 18.2 mmol) in 99.5% ethanol (40 mL) was stirred under reflux for 20 h. The solvent was removed, and the residue was purified by silica gel flash chromatography (ethyl acetate/methanol 9:1) to give the product as a white solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541592B2uspto-grants-2013_09