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Potassium Carbonate → Methyl methoxyimino-[2-(3-methoxyimino-2,3-dihydrobenzofuran-6-yloxymethyl)-phenyl]acetate

HRID 2184647
ノート
印刷プレビュー

反応式

HRID 2184647 の反応式
[CH3:1][O:2][N:3]=[C:4]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[CH2:15]Br)[C:5]([O:7][CH3:8])=[O:6].C(=O)([O-])[O-].[K+].[K+].[CH3:23][O:24][N:25]=[C:26]1[C:30]2[CH:31]=[CH:32][C:33]([OH:35])=[CH:34][C:29]=2[O:28][CH2:27]1>CN(C)C=O>[CH3:1][O:2][N:3]=[C:4]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[CH2:15][O:35][C:33]1[CH:32]=[CH:31][C:30]2[C:26](=[N:25][O:24][CH3:23])[CH2:27][O:28][C:29]=2[CH:34]=1)[C:5]([O:7][CH3:8])=[O:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 54028047Methyl 2-[2-(bromomethyl)phenyl]-2-(methoxyimino)acetateHCID 1359949623-Methoxyimino-6-hydroxy-2,3-dihydrobenzofuran

生成物 1

HCID 86757390Methyl methoxyimino-[2-(3-methoxyimino-2,3-dihydrobenzofuran-6-yloxymethyl)-phenyl]acetate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

3.4 g of (E) methyl methoxyimino-(2-bromomethylphenyl)acetate was added to 9.0 g of potassium carbonate and 1.8 g of 3-methoxyimino-6-hydroxy-2,3-dihydrobenzofuran in 30 ml of N,N-dimethylformamide, and they were reacted at room temperature for 6 hours. After the completion of the reaction, the reaction liquid was poured in ice/water. After the extraction with ethyl acetate, the extract was washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue thus obtained was purified by the silica gel chromatography (hexane:ethyl acetate) to obtain 3.0 g of the title compound. (having a m.p. of 108-110° C. and 1H-NMR data shown in the following table).

後処理

  1. customwere reacted at room temperature for 6 hours
  2. customAfter the completion of the reaction
  3. customthe reaction liquid
  4. extractionAfter the extraction with ethyl acetate
  5. washthe extract was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe residue thus obtained
  9. customwas purified by the silica gel chromatography (hexane:ethyl acetate)

出典と根拠

ORDレコード
ord-db6a9d669642469180d8cc6491ba8da5
出典データセット
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06399542B1

反応ノート

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