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Water → HCID 57296520、化合物

HRID 1905399
ノート
印刷プレビュー

反応式

HRID 1905399 の反応式
[Cl:1][C:2]1[CH:18]=[CH:17][C:5]([O:6][C:7]2[N:11]([CH3:12])[N:10]=[C:9]([CH3:13])[C:8]=2[CH:14]=[N:15][OH:16])=[CH:4][CH:3]=1.[OH-].[Na+].Br[CH2:22][C:23]1[CH:32]=[CH:31][CH:30]=[CH:29][C:24]=1[C:25]([O:27][CH3:28])=[O:26].O>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:6][C:7]2[N:11]([CH3:12])[N:10]=[C:9]([CH3:13])[C:8]=2[CH:14]=[N:15][O:16][CH2:22][C:23]2[CH:32]=[CH:31][CH:30]=[CH:29][C:24]=2[C:25]([O:27][CH3:28])=[O:26])=[CH:17][CH:18]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 12148555-(4-Chlorophenoxy)-1,3-dimethyl-1H-pyrazole-4-carboxaldehyde oximeHCID 2734813Methyl 2-(bromomethyl)benzoate

生成物 1

HCID 57296520HCID 57296520、化合物収率 64%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

2.0 Grams (0.00755 mole) of 5-(4-chlorophenoxy)-1,3-dimethyl-pyrazole-4-carbaldehyde oxime was dissolved in 20 ml of dimethylformamide, and after adding 0.5 g (0.0125 mole) of powdery sodium hydroxide, the resulting mixture was thoroughly stirred. To this solution was added 1.73 g (0.00755 mole) of methyl 2-bromomethylbenzoate, and reaction was carried out at from 70° to 80° C. for 5 hours. After completion of the reaction, water was added to the reaction solution which was then extracted with ethyl acetate. The ethyl acetate extract was washed with water and dried, and ethyl acetate was removed by evaporation to obtain an oily product. This oily product was column-chromatographed on silica gel to obtain 2.0 g cf the desired compound.

後処理

  1. additionTo this solution was added
  2. additionwas added to the reaction solution which
  3. extractionwas then extracted with ethyl acetate
  4. extractionThe ethyl acetate extract
  5. washwas washed with water
  6. customdried
  7. customethyl acetate was removed by evaporation
  8. customto obtain an oily product
  9. customThis oily product was column-chromatographed on silica gel

出典と根拠

ORDレコード
ord-8e2f7b376ba54bddb235da80c47af322
出典データセット
uspto-grants-1989_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04843068

反応ノート

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