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HCID 629261、化合物 → HCID 14547484、化合物

HRID 979576
ノート
印刷プレビュー

反応式

HRID 979576 の反応式
[C:1]([C:4]1[CH:5]=[CH:6][C:7]2[C:11](Br)=[C:10](Br)[S:9][C:8]=2[CH:14]=1)(=[O:3])[CH3:2]>C(O)C.C(OCC)(=O)C>[C:1]([C:4]1[CH:5]=[CH:6][C:7]2[CH:11]=[CH:10][S:9][C:8]=2[CH:14]=1)(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 629261HCID 629261、化合物

生成物 1

HCID 14547484HCID 14547484、化合物収率 107.8%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

6-Acetyl-2,3-dibromobenzo[b]thiophene (6.68 g, 20 mmole) was dissolved in a mixture of ethanol and ethyl acetate (100 ml each) and MgO (1.6 g) and (20% Pd(OH2)/C (800 mg) were added under a N2 atmosphere. Hydrogenolysis was carried out at 40 psi of H2 at room temperature for 3 hours. The catalyst was removed by filtration and the solvent was removed in vacuo. The residue was partitioned between CHCl3 (100 ml) and H2O (50 ml). The CHCl3 layer was washed with H2O (50 ml). The aqueous layers were combined and back-extracted with CHCl3 (30 ml). The CHCl3 solutions were combined, dried over Na2SO4 and the solvent evaporated in vacuo to yield 3.8 g of product which was used in the next step without further purification.

後処理

  1. customThe catalyst was removed by filtration
  2. customthe solvent was removed in vacuo
  3. customThe residue was partitioned between CHCl3 (100 ml) and H2O (50 ml)
  4. washThe CHCl3 layer was washed with H2O (50 ml)
  5. extractionback-extracted with CHCl3 (30 ml)
  6. dry with materialdried over Na2SO4
  7. customthe solvent evaporated in vacuo

出典と根拠

ORDレコード
ord-77f070222e4c441db19e7afe4a7ac116
出典データセット
uspto-grants-1987_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04668697

反応ノート

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