Pyrazole → HCID 69743545、化合物

HRID 1760374ノート

反応式

HRID 1760374 の反応式
[CH2:1]([O:3][C:4]([C:6]1([C:27]([O:29][CH2:30][CH3:31])=[O:28])[CH2:10][CH2:9][C:8](=[O:11])[N:7]1[C:12]1[CH:13]=[N:14][C:15]([O:18][C:19]2[CH:24]=[CH:23][C:22]([CH2:25]Br)=[CH:21][CH:20]=2)=[CH:16][CH:17]=1)=[O:5])[CH3:2].[NH:32]1[CH:36]=[CH:35][CH:34]=[N:33]1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O.O>[CH2:1]([O:3][C:4]([C:6]1([C:27]([O:29][CH2:30][CH3:31])=[O:28])[CH2:10][CH2:9][C:8](=[O:11])[N:7]1[C:12]1[CH:13]=[N:14][C:15]([O:18][C:19]2[CH:24]=[CH:23][C:22]([CH2:25][N:32]3[CH:36]=[CH:35][CH:34]=[N:33]3)=[CH:21][CH:20]=2)=[CH:16][CH:17]=1)=[O:5])[CH3:2]

参加物

6

反応物 3

HCID 1048PyrazoleHCID 11430Potassium CarbonateHCID 69741938HCID 69741938、化合物

生成物 1

HCID 69743545HCID 69743545、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

To a solution of 1-[6-(4-bromomethyl-phenoxy)-pyridin-3-yl]-5-oxo-pyrrolidine-2,2-dicarboxylic acid diethyl ester (0.2 g, 0.4 mmol) in 0.8 mL of dimethylformamide was added pyrazole (0.056 g, 0.82 mmol) and potassium carbonate (0.11 g, 0.82 mmol). After stirring for 24 hours at 50° C., the mixture was diluted with water, extracted three times with ethyl acetate, and the combined organic phases were dried over sodium sulfate, filtered and concentrated in vacuo, affording the crude product as a colorless syrup that was used directly in the next step. MS (APCl, m/z): 479.2 [M+H]+.

後処理

  1. extractionextracted three times with ethyl acetate
  2. dry with materialthe combined organic phases were dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-7b193e426e9c4c84b49a81ace2b50911
出典データセット
uspto-grants-2005_01
特許番号
US06841671B2

反応ノート

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