Potassium Carbonate → 1-[2-(4-tert-butyl-phenyl)-2-oxo-ethyl]-1H-pyrazole-3,5-dicarboxylic acid diethyl ester

HRID 2272952ノート

反応式

HRID 2272952 の反応式
[NH:1]1[C:5]([C:6]([O:8][CH2:9][CH3:10])=[O:7])=[CH:4][C:3]([C:11]([O:13][CH2:14][CH3:15])=[O:12])=[N:2]1.Br[CH2:17][C:18]([C:20]1[CH:25]=[CH:24][C:23]([C:26]([CH3:29])([CH3:28])[CH3:27])=[CH:22][CH:21]=1)=[O:19].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH2:9]([O:8][C:6]([C:5]1[CH:4]=[C:3]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[N:2]([CH2:17][C:18]([C:20]2[CH:25]=[CH:24][C:23]([C:26]([CH3:29])([CH3:28])[CH3:27])=[CH:22][CH:21]=2)=[O:19])[N:1]=1)=[O:7])[CH3:10]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 142184diethyl 1H-pyrazole-3,5-dicarboxylateHCID 23247702-Bromo-1-(4-tert-butylphenyl)ethan-1-one

生成物 1

HCID 898321591-[2-(4-tert-butyl-phenyl)-2-oxo-ethyl]-1H-pyrazole-3,5-dicarboxylic acid diethyl ester

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A solution of 849 mg (4.00 mmol) diethyl pyrazole-3,5-dicarboxylate and 1.02 g (4.00 mmol) 2-bromo-1-(4-tert-butyl-phenyl)-ethanone in 4 ml acetone is treated with 663 mg (4.80 mmol) potassium carbonate. The resulting suspension is stirred overnight at room temperature. The reaction mixture is partitioned between water and dichloromethane. The organic phase is dried over sodium sulfate and evaporated to give 1-[2-(4-tert-butyl-phenyl)-2-oxoethyl]-1H-pyrazole-3,5-dicarboxylic acid diethyl ester as light yellow foam; HPLC/MS 2.77 (A), [M+H] 387.

後処理

  1. customThe reaction mixture is partitioned between water and dichloromethane
  2. dry with materialThe organic phase is dried over sodium sulfate
  3. customevaporated

出典と根拠

ORDレコード
ord-51afb1646a694c9c8bde1f93671bab3e
出典データセット
uspto-grants-2015_09
特許番号
US09120805B2

反応ノート

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