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Sodium borohydride → 6-Methoxy-1-benzothiophene

HRID 507684
ノート
印刷プレビュー

反応式

HRID 507684 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[C:10](=O)[CH2:9][S:8][C:7]=2[CH:12]=1.[BH4-].[Na+]>CO.[OH-].[Na+]>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[CH:10]=[CH:9][S:8][C:7]=2[CH:12]=1
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 2

HCID 4311764Sodium borohydrideHCID 121016256-Methoxybenzo[B]thiophen-3(2H)-one

生成物 1

HCID 136342376-Methoxy-1-benzothiophene収率 66.1%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 14798Sodium Hydroxide溶媒2 回

実験手順

6-Methoxybenzo[b]thiophen-3(2H)-one (1.4 g, 7.76 mmol) was dissolved in a mixture of methanol (18 mL) and 2.5 M sodium hydroxide (3 mL). The mixture was treated with sodium borohydride (0.589 g, 15 mmol) in 10 mL of methanol and 3 mL of 2.5 M sodium hydroxide. The reflux was heated to reflux for 1 h and then at 60° C. overnight. The reaction was cooled down to room temperature and the methanol removed in vacuo. The remaining aqueous layer was acidified to pH 4 with 1 N hydrochloric acid. The aqueous layer was extracted with ethyl acetate and washed with 1 N HCl. The organic layer was further washed with water, saturated sodium bicarbonate, water and brine. The organic layer was dried with sodium sulfate, concentrated and purified by flash chromatography usng a gradient of 20 to 50% ethyl acetate in hexanes to afford a clear oil (0.843 g).

後処理

  1. temperatureThe reflux was heated
  2. temperatureto reflux for 1 h
  3. customat 60° C.
  4. customovernight
  5. customthe methanol removed in vacuo
  6. extractionThe aqueous layer was extracted with ethyl acetate
  7. washwashed with 1 N HCl
  8. washThe organic layer was further washed with water, saturated sodium bicarbonate, water and brine
  9. dry with materialThe organic layer was dried with sodium sulfate
  10. concentrationconcentrated
  11. custompurified by flash chromatography

出典と根拠

ORDレコード
ord-79b1d4e6ffc8444688f13ea1be1bc5af
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07786132B2

反応ノート

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