反応 #632020

ord-db179f7c42db4ba0b5e0c3cd9209b495

反応方程式

C1CN2CCC(CC2)N1
1,4-diazabicyclo[3.2.2]nonane
O=[N+]([O-])c1cnc(Cl)nc1
2-chloro-5-nitro-pyrimidine
O=C([O-])O.[Na+]
sodium bicarbonate
O=[N+]([O-])c1cnc(N2CCN3CCC2CC3)nc1
4-(5-Nitro-pyrimidin-2-yl)-1,4-diaza-bicyclo[3.2.2]nonane

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出followed by extraction with ethylacetate (3×20 ml)
  2. 2
    その他The organic phase was dried
  3. 3
    その他evaporated
  4. 4
    その他a yellow powder was isolated

実験手順

A mixture of 1,4-diazabicyclo[3.2.2]nonane (0.87 g, 6.90 mmol), 2-chloro-5-nitro-pyrimidine (1.56 g, 6.27 mmol) and dioxane (75 ml) was stirred at room-temperature for 15 h. Aqueous sodium bicarbonate (20 ml, 10%) was added followed by extraction with ethylacetate (3×20 ml). The organic phase was dried and evaporated and a yellow powder was isolated. Yield 0.86 g (55%). Mp 135-139° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07935695B2uspto-grants-2011_05