Triethylamine → 5-Chloro-2-(trifluoromethyl)pyrimidine

HRID 852395

反応式

HRID 852395 の反応式
[F:1][C:2]([F:7])([F:6])[C:3]([NH2:5])=[NH:4].[Cl:8]/[C:9](=[CH:14]\N(C)C)/[CH:10]=[N+](C)C.CCN1C2C(S/C/1=C\C#C/C(/C)=C\C1SC3C(=CC=CC=3)[N+]=1CC)=CC=CC=2.F[P-](F)(F)(F)(F)F.C(N(CC)CC)C>C(#N)C.O>[Cl:8][C:9]1[CH:10]=[N:4][C:3]([C:2]([F:7])([F:6])[F:1])=[N:5][CH:14]=1

参加物

7

反応物 4

HCID 8471TriethylamineHCID 2776882TrifluoroacetamidineHCID 6477909Hexafluoro phosphateHCID 10590808HCID 10590808、化合物

生成物 1

HCID 336979605-Chloro-2-(trifluoromethyl)pyrimidine収率 56.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

実験手順

A solution of 4.70 g (85% purity, 35.65 mmol) of trifluoroacetamidine and 10.93 g (35.65 mmol) of ((Z)-2-chloro-3-dimethylamino-allylidene)-dimethyl-ammonium; hexafluoro phosphate [Davies, Ian W.; Marcoux, Jean-Francois; Wu, Jimmy; Palucki, Michael; Corley, Edward G.; Robbins, Michael A.; Tsou, Nancy, Ball, Richard G.; Dormer, Peter; Larsen, Robert D.; Reider, Paul J, Journal of Organic Chemistry 2000, 65(15), 4571-4574] in 70 ml acetonitrile was treated with 4.33 ml (42.78 mol) of triethylamine and stirred for 4 h at room temperature. The reaction was poured into 250 ml of water and extracted with ether (three times). The organic phases were washed with water (two times), dried (Na2SO4) and carefully evaporated to give 3.66 g of the title compound as an orange volatile liquid.

後処理

  1. extractionextracted with ether (three times)
  2. washThe organic phases were washed with water (two times)
  3. dry with materialdried (Na2SO4)
  4. customcarefully evaporated

出典と根拠

ORDレコード
ord-7671513651e443afa296bc72042681e4
出典データセット
uspto-grants-2007_08
特許番号
US07253192B2

関連ノート

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