Methanol → 2-(4-Nitrophenyl)butanol

HRID 1074442

反応式

HRID 1074442 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([CH:10]([CH2:14][CH3:15])[C:11](O)=[O:12])=[CH:6][CH:5]=1)([O-:3])=[O:2].CO>O1CCCC1>[N+:1]([C:4]1[CH:5]=[CH:6][C:7]([CH:10]([CH2:14][CH3:15])[CH2:11][OH:12])=[CH:8][CH:9]=1)([O-:3])=[O:2]

参加物

4

反応物 2

HCID 887MethanolHCID 240472-(4-Nitrophenyl)butyric acid

生成物 1

HCID 204966922-(4-Nitrophenyl)butanol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of 20.9 g of 2-(4-nitrophenyl)butyric acid in 500 ml of dry tetrahydrofuran was added, dropwise, 1.1 equivalents of 10 M borane-dimethylsulfide complex in 100 ml of dry tetrahydrofuran. The mixture was stirred at room temperature for 1.5 hours and then refluxed for 1.5 hours and finally cooled to room temperature. Methanol (10 ml) was added, the mixture was stirred for 30 minutes, and the solvent was then evaporated under reduced pressure. The residue was dissolved in 100 ml of methanol and the solvent was evaporated and this procedure was repeated three (3) times. The resulting oil was purified by chromatography on silica gel, eluting with 1:1 ethyl acetate/hexane to give 2-(4-nitrophenyl)butanol as a light-yellow oil.

後処理

  1. temperaturerefluxed for 1.5 hours
  2. temperaturefinally cooled to room temperature
  3. stirringthe mixture was stirred for 30 minutes
  4. customthe solvent was then evaporated under reduced pressure
  5. dissolutionThe residue was dissolved in 100 ml of methanol
  6. customthe solvent was evaporated
  7. customThe resulting oil was purified by chromatography on silica gel
  8. washeluting with 1:1 ethyl acetate/hexane

出典と根拠

ORDレコード
ord-b7075177e6024583b3104666f58b59d3
出典データセット
uspto-grants-1983_07
特許番号
US04391818

関連ノート

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