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

HRID 852395

반응식

HRID 852395 반응식
[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

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 2776882TrifluoroacetamidineHCID 6477909Hexafluoro phosphateHCID 10590808HCID 10590808, 화합물

생성물 1

HCID 336979605-Chloro-2-(trifluoromethyl)pyrimidine수율 56.2%

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-7671513651e443afa296bc72042681e4
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07253192B2

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