反応 #1265404

ord-de7d23d797264dddbff92aba1d132db1

反応方程式

Nc1cc(O)nc(N)n1
2,6-diamino-4-hydroxypyrimidine
CC(=O)O
acetic acid
O=N[O-].[Na+]
NaNO2
Nc1nc(N)c(N=O)c(O)n1
title compound
収率 97.3%
Nc1nc(N)c(N=O)c(O)n1
2,6-diamino-5-nitroso-4-hydroxypyrimidine
収率 97.3%

反応条件

温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他A pink precipitate was formed
  2. 2
    温度The reaction mixture was cooled down in the refrigerator overnight
  3. 3
    ろ過The precipitate was filtered off
  4. 4
    乾燥dried over P2O5

実験手順

To a solution of 2,6-diamino-4-hydroxypyrimidine (12.9 g, 102.2 mmoles) in 200 ml of a 10% acetic acid solution in water at 80° C. was added dropwise a solution of NaNO2 (7.05 g, 102.2 mmoles) in 20 ml water. A pink precipitate was formed, which was further stirred for 1 hour at 80° C. The reaction mixture was cooled down in the refrigerator overnight. The precipitate was filtered off and dried over P2O5, providing the title compound as a pink powder (15.43 g, yield: 97%). The spectral data are in accordance with literature data (Landauer et al. in J. Chem. Soc. (1953) 3721–3722).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07276506B2uspto-grants-2007_10