反应 #162634

ord-451997b8ecc143308e17e807e39f5ea7

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The reaction
  2. 2
    其他a white precipitate formed
  3. 3
    温度the mixture was refluxed for three days
  4. 4
    温度The reaction was cooled
  5. 5
    其他to precipitate a white solid
  6. 6
    过滤The solids were collected by filtration
  7. 7
    洗涤washed with diethyl ether

实验过程

To a solution of 2,4,5,6-tetrachloro-pyrimidine (2.0 g, 9.2 mmol) in THF (20 mL) and triethylamine (excess) was added 3-oxa-8-aza-bicyclo[3.2.1]octane (2.7 g, 18 mmol) at −78° C. The reaction slowly warmed to room temperature and a white precipitate formed. To the reaction was added water (2.0 mL) and the mixture was refluxed for three days. The reaction was cooled and water was added to precipitate a white solid. The solids were collected by filtration and washed with diethyl ether to yield the title compound (2.0 g). MS m/z=372 (M+H).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08835429B2uspto-grants-2014_09