[2,6-Dichloro-4-(trifluoromethyl)phenyl]hydrazine → Methyl 1-(2,6-dichloro-4-trifluoromethylphenyl)-3,5-diethylpyrazole4-carboxylate

HRID 1740095노트

반응식

HRID 1740095 반응식
[CH3:1][O:2][C:3]([CH:5]([C:10](=O)[CH2:11][CH3:12])[C:6](=O)[CH2:7][CH3:8])=[O:4].[Cl:14][C:15]1[CH:20]=[C:19]([C:21]([F:24])([F:23])[F:22])[CH:18]=[C:17]([Cl:25])[C:16]=1[NH:26][NH2:27]>C(O)C>[Cl:14][C:15]1[CH:20]=[C:19]([C:21]([F:23])([F:22])[F:24])[CH:18]=[C:17]([Cl:25])[C:16]=1[N:26]1[C:10]([CH2:11][CH3:12])=[C:5]([C:3]([O:2][CH3:1])=[O:4])[C:6]([CH2:7][CH3:8])=[N:27]1

참가 물질

4

반응물 2

HCID 688223[2,6-Dichloro-4-(trifluoromethyl)phenyl]hydrazineHCID 21837307Methyl 3-oxo-2-propionylpentanoate

생성물 1

HCID 21837355Methyl 1-(2,6-dichloro-4-trifluoromethylphenyl)-3,5-diethylpyrazole4-carboxylate수율 43%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 7.5 g (40 mmol) of the compound of step A and 11.85 g (48 mmol) of 2,6-dichloro-4-trifluoromethylphenyl hydrazine in 50 mL of ethanol was heated at reflux for 8 hours. The ethanol was removed by evaporation and the residues were partitioned between ethyl acetate and dilute hydrogen chloride. The organic extracts were dried and evaporated to give the desired product in 43% yield as a maroon oil. 1H-NMR (CDCl3) δ 1.08 (3H, t, J=7), 1.24 (3H, t, J=7), 2.22 (2H, q, J=7), 2.58 (4H, q. J=7), J=7), 3.86 (3H, s), 7.46 (2H, s).

후처리

  1. temperatureat reflux for 8 hours
  2. customThe ethanol was removed by evaporation
  3. customthe residues were partitioned between ethyl acetate and dilute hydrogen chloride
  4. customThe organic extracts were dried
  5. customevaporated

출처 및 근거

ORD 기록
ord-e6d5b5263c784764a16086980d5347be
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05968944

반응 노트

불러오는 중…