Hydrochloric Acid → HCID 22618361, 화합물

HRID 861255노트

반응식

HRID 861255 반응식
[CH3:1][Mg]I.[Cl:4][C:5]1[CH:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:8]=[C:7]([Cl:15])[C:6]=1[N:16]1[CH:20]=C(C#N)[C:18]([C:23]([F:26])([F:25])[F:24])=[N:17]1.Cl.C([O:30][CH2:31][CH3:32])C>>[C:31]([C:32]1[C:18]([C:23]([F:26])([F:24])[F:25])=[N:17][N:16]([C:6]2[C:7]([Cl:15])=[CH:8][C:9]([C:11]([F:13])([F:14])[F:12])=[CH:10][C:5]=2[Cl:4])[CH:20]=1)(=[O:30])[CH3:1]

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 3283Diethyl Ether2회HCID 14280195HCID 14280195, 화합물HCID 178418373HCID 178418373, 화합물

생성물 1

HCID 22618361HCID 22618361, 화합물

실험 절차

A solution of methylmagnesium iodide (prepared from magnesium (0.26 g) and methyl iodide (1.5 g) in diethyl ether (25 ml)), was treated with a solution of 1-(2,6-dichloro-4-trifluoromethylphenyl)-4-cyano-3-trifluoromethylpyrazole (2 g) in diethyl ether (20 ml), dropwise. The resulting pale yellow solution was refluxed for 24 hours, cooled, and treated with hydrochloric acid (2N, 10 ml). After stirring for 0.5 hour at room temperature, the reaction mixture was diluted with ether (50 ml). The ethereal extract was washed with water (50 ml), dried over anhydrous magnesium sulphate, and evaporated in vacuo to give a yellow gum. This was purified by chromatography on silica (Merck, 200-400 mesh, 0.7 kg cm-2) eluting with a mixture of dichloromethane and petroleum ether (4:1) to give 4-acetyl-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-trifluoromethylpyrazole as a white solid, m.p. 134° C.

후처리

  1. temperatureThe resulting pale yellow solution was refluxed for 24 hours
  2. temperaturecooled
  3. extractionThe ethereal extract
  4. washwas washed with water (50 ml)
  5. dry with materialdried over anhydrous magnesium sulphate
  6. customevaporated in vacuo
  7. customto give a yellow gum
  8. customThis was purified by chromatography on silica (Merck, 200-400 mesh, 0.7 kg cm-2)
  9. washeluting with a mixture of dichloromethane and petroleum ether (4:1)

출처 및 근거

ORD 기록
ord-0a7a2cdadaa64e9c89f904a2446ef8cd
출처 데이터셋
uspto-grants-1998_02
특허 번호
US05714191

반응 노트

불러오는 중…