反応 #95000

ord-332f755aa4f94c26b724fcd1f0380f00

反応方程式

N=C(N)C(Cl)(Cl)Cl
trichloroacetamidine
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CCOC(=O)CC(=O)CCl
ethyl-4-chloroacetoacetate
Oc1cc(CCl)nc(C(Cl)(Cl)Cl)n1
crude product
収率 36.1%
Oc1cc(CCl)nc(C(Cl)(Cl)Cl)n1
6-Chloromethyl-4-Hydroxy-2-Trichloromethylpyrimidine
収率 36.1%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過The aqueous solution was filtered
  2. 2
    その他to give a precipitate
  3. 3
    洗浄The precipitate was washed
  4. 4
    その他dried

実験手順

A mixture of 30.0 g (0.18 mole) trichloroacetamidine, 25.2 g (0.18 mole) potassium carbonate, 30.3 g (0.18 mole) ethyl-4-chloroacetoacetate and 400 ml water was stirred 18 hours. The aqueous solution was filtered and acidified with hydrochloric acid to give a precipitate. The precipitate was washed and dried to give 17.0 g (36% yield) of crude product. An analytical sample recrystallized from ligroin had mp 138°-144° C. The structure was confirmed via infrared and elemental analysis.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04343803uspto-grants-1982_08