Ethyl Acetate → (1-ethylpyrazol-5-yl) 2,4-dichloro-3-(1-methyl-3-methylcarbonyl-1H-pyrazol-5-yl)benzoate

HRID 1276127

反応式

HRID 1276127 の反応式
[CH2:1]([N:3]1[C:7]([OH:8])=[CH:6][CH:5]=[N:4]1)[CH3:2].[Cl:9][C:10]1[C:18]([C:19]2[N:23]([CH3:24])[N:22]=[C:21]([C:25]([CH3:27])=[O:26])[CH:20]=2)=[C:17]([Cl:28])[CH:16]=[CH:15][C:11]=1[C:12](O)=[O:13].C(=O)([O-])[O-].[Na+].[Na+].C(OCC)(=O)C>C(#N)C>[Cl:9][C:10]1[C:18]([C:19]2[N:23]([CH3:24])[N:22]=[C:21]([C:25]([CH3:27])=[O:26])[CH:20]=2)=[C:17]([Cl:28])[CH:16]=[CH:15][C:11]=1[C:12]([O:8][C:7]1[N:3]([CH2:1][CH3:2])[N:4]=[CH:5][CH:6]=1)=[O:13]

参加物

6

反応物 4

HCID 8857Ethyl AcetateHCID 10340Sodium CarbonateHCID 221149072,4-dichloro-3-(1-methyl-3-methylcarbonyl-1H-pyrazol-5-yl)benzoic acidHCID 178418331HCID 178418331、化合物

生成物 1

HCID 53727367(1-ethylpyrazol-5-yl) 2,4-dichloro-3-(1-methyl-3-methylcarbonyl-1H-pyrazol-5-yl)benzoate収率 27.1%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

0.21 g (1.9 mmol) of 1-ethyl-5-hydroxy-1H-pyrazole and 0.39 g (1.9 mmol) of N,N-dicyclohexylcarbodiimide were added to 0.59 g (1.9 mmol) of 2,4-dichloro-3-(1-methyl-3-methylcarbonyl-1H-pyrazol-5-yl)benzoic acid in 8 ml of acetonitrile. The mixture was stirred at room temperature for 12 hours and 25 ml of 5% strength sodium carbonate solution and 50 ml of ethyl acetate were added, insoluble components were filtered off and the organic phase was separated off, dried and concentrated. The residue was subsequently chromatographed over silica gel (eluent: ethyl acetate:cyclohexane=1:1). 0.21 g (27% of theory) of (1-ethylpyrazol-5-yl) 2,4-dichloro-3-(1-methyl-3-methylcarbonyl-1H-pyrazol-5-yl)benzoate was obtained.

後処理

  1. filtrationinsoluble components were filtered off
  2. customthe organic phase was separated off
  3. customdried
  4. concentrationconcentrated
  5. customThe residue was subsequently chromatographed over silica gel (eluent: ethyl acetate:cyclohexane=1:1)

出典と根拠

ORDレコード
ord-01b944fcd4c8489082f50d481062d0ff
出典データセット
uspto-grants-2000_12
特許番号
US06165944

関連ノート

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