反応 #2298641

ord-a60e2284ddd343c7998f755014dbc362

反応方程式

CCc1nc(C)cc(=O)n1CCOc1ccc(CNO)cc1
4-[2-[2-ethyl-4-methyl-6-oxo-1,6dihydro-1-pyrimidinyl]ethoxy]benzyl hydroxylamine
N#C[O][K]
KOCN
CCc1nc(C)cc(=O)n1CCOc1ccc(CN(O)C(N)=O)cc1
compound
収率 85.2%
CCc1nc(C)cc(=O)n1CCOc1ccc(CN(O)C(N)=O)cc1
N-[4-[2-[2-Ethyl-4-methyl-6-oxo-1,6-dihydro-1-pyrimidinyl]ethoxy]benzyl]N-hydroxyurea
収率 85.2%

反応条件

温度
30°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted with ethyl acetate (3×10 ml)
  2. 2
    洗浄The combined organic layers were washed with brine
  3. 3
    乾燥dried over anhydrous Na2SO4
  4. 4
    濃縮concentrated

実験手順

To a stirred solution of 4-[2-[2-ethyl-4-methyl-6-oxo-1,6dihydro-1-pyrimidinyl]ethoxy]benzyl hydroxylamine (303 mg, 1.0 mmol) (obtained from preparation 18) in a mixture of water (2 ml) and acetic acid (0.5 ml) was added a solution of KOCN (343 mg, 3.0 mmol) in water (1 ml) and stirred for 1 h at 30° C. The reaction mixture was diluted with water and extracted with ethyl acetate (3×10 ml). The combined organic layers were washed with brine, dried over anhydrous Na2SO4 and concentrated to yield the compound (295 mg, 85%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: USRE039266E1uspto-grants-2006_09