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Sodium borohydride → 4-Bromo-6-fluoro-2,3-dihydro-1H-inden-1-ol

HRID 574633
ノート
印刷プレビュー

反応式

HRID 574633 の反応式
[Br:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[C:7]2[C:3]=1[CH2:4][CH2:5][C:6]2=[O:12].[BH4-].[Na+]>C(O)C>[Br:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[C:7]2[C:3]=1[CH2:4][CH2:5][CH:6]2[OH:12]
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 2

HCID 4311764Sodium borohydrideHCID 117702304-bromo-6-fluoro-2,3-dihydro-1H-inden-1-one

生成物 1

HCID 894444374-Bromo-6-fluoro-2,3-dihydro-1H-inden-1-ol収率 99%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

According to Scheme 2, step 1: To a solution of 4-Bromo-6-fluoro-indan-1-one (10.0 g, 43.7 mmol) in ethanol (183 ml) at 0° C. NaBH4 (3.67 g, 97.0 mmol) was added in portions and then the mixture was stirred at room temperature for 18 h. After evaporation of solvents in vacuo, water was added to the residue, the solution was extracted 3 times with ethyl acetate, then 2N aqueous HCl was added and the combined organic layers were washed with saturated aq. NaHCO3 and water. After drying over Na2SO4 and filtration, solvents were evaporated in vacuo to give 10.0 g of 4-Bromo-6-fluoro-indan-1-ol (4a) which was used immediately in the next step without purification.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. customat 0° C
  2. customAfter evaporation of solvents in vacuo, water
  3. additionwas added to the residue
  4. extractionthe solution was extracted 3 times with ethyl acetate
  5. addition2N aqueous HCl was added
  6. washthe combined organic layers were washed with saturated aq. NaHCO3 and water
  7. dry with materialAfter drying over Na2SO4 and filtration, solvents
  8. customwere evaporated in vacuo

出典と根拠

ORDレコード
ord-d79fef12805943159f06ba839ae774d5
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09034897B2

反応ノート

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