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

HRID 1740095ノート

反応式

HRID 1740095 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-e6d5b5263c784764a16086980d5347be
出典データセット
uspto-grants-1999_10
特許番号
US05968944

反応ノート

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