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Ethanol → HCID 11138604、化合物

HRID 487794
ノート
印刷プレビュー

反応式

HRID 487794 の反応式
C(O)C.[Cl:4][C:5]1[C:10]([CH3:11])=[C:9](Br)[CH:8]=[C:7]([S:13]([CH3:16])(=[O:15])=[O:14])[C:6]=1[CH3:17].C([O-])(=O)C.[Na+].[H][H]>[Pd].O>[Cl:4][C:5]1[C:6]([CH3:17])=[C:7]([S:13]([CH3:16])(=[O:15])=[O:14])[CH:8]=[CH:9][C:10]=1[CH3:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 702EthanolHCID 517045Sodium AcetateHCID 10859468HCID 10859468、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 11138604HCID 11138604、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 962
Water
溶媒

実験手順

30 ml of ethanol was added to 1.0 g of the crude 2-chloro-4-bromo-6-methylsulfonyl-m-xylene obtained in Example 3, and 0.1 g of 5% palladium active carbon and 1.0 g of anhydrous sodium acetate were further added thereto. The reactor was sealed, and was substituted with hydrogen, then stirring at room temperature for 7 hours. 30 ml of water was added to the reaction liquor, and was concentrated under reduced pressure. 30 ml of EDC was further added thereto, and the resultant mixture was filtered. The EDC layer was taken out from the filtrate, and was washed with 20 ml of water and then with 10 ml of a saturated aqueous solution of common salt, and was dried over anhydrous sodium sulfate. The EDC layer thus obtained was concentrated under reduced pressure and was dried to a solid to obtain 0.7 g of a crude product of the above-identified aimed compound (purity measured by gas chromatography: 75.6%). The crude product thus obtained was recrystallized by methanol to obtain the above-identified aimed compound.

後処理

  1. additionwere further added
  2. customThe reactor was sealed
  3. concentrationwas concentrated under reduced pressure
  4. addition30 ml of EDC was further added
  5. filtrationthe resultant mixture was filtered
  6. washwas washed with 20 ml of water
  7. dry with materialwith 10 ml of a saturated aqueous solution of common salt, and was dried over anhydrous sodium sulfate
  8. customThe EDC layer thus obtained
  9. concentrationwas concentrated under reduced pressure
  10. customwas dried to a solid
  11. customto obtain 0.7 g of a crude product of the above-identified aimed compound (purity measured by gas chromatography: 75.6%)
  12. customThe crude product thus obtained
  13. customwas recrystallized by methanol

出典と根拠

ORDレコード
ord-928e2cbb01ad43e48f23c6e7312ebf2f
出典データセット
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05296634

反応ノート

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