Hydrochloric Acid → HCID 178418429, 화합물

HRID 1813

반응식

HRID 1813 반응식
[C:1]([C:3]1[C:7]([S:8][C:9]([F:12])([F:11])[F:10])=[C:6]([NH:13]C(=O)C(F)(F)F)[NH:5][N:4]=1)#[N:2].[OH-].[NH4+].Cl>CO.C(OCC)(=O)C>[C:1]([C:3]1[C:7]([S:8][C:9]([F:12])([F:11])[F:10])=[C:6]([NH2:13])[NH:5][N:4]=1)#[N:2]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14923Ammonium HydroxideHCID 1784183603-cyano-4-trifluoromethylsulfenyl-5-(N-trifluoroacetylamino)pyrazole

생성물 1

HCID 178418429HCID 178418429, 화합물수율 87.6%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

The product of Step E (55 g, 181 mmoles) was dissolved in methanol. 100 ml of ammonium hydroxide were added, the solution was refluxed for 3 hours and then stirred at room temperature for 15 hours. The methanolic solution was brought to pH7 using concentrated aqueous hydrochloric acid and diluted with ethyl acetate. The organic layer was washed several times with water and brine, dried over MgSO4 and concentrated to dryness to give an oily brown residue which was recrystallized from methyl tert-butyl ether to afford 33 g of the title compound, m.p. around 187° C.

후처리

  1. temperaturethe solution was refluxed for 3 hours
  2. washThe organic layer was washed several times with water and brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated to dryness
  5. customto give an oily brown residue which
  6. customwas recrystallized from methyl tert-butyl ether

출처 및 근거

ORD 기록
ord-519d1ed0c254438c8f86070fac54bfc1
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05726324

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