4-Nitrosalicylic acid → 2-Hydroxy-4-nitrobenzyl alcohol

HRID 15445ノート

反応式

HRID 15445 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([OH:13])[C:7](=[CH:11][CH:12]=1)[C:8](O)=[O:9])([O-:3])=[O:2]>C1COCC1>[OH:9][CH2:8][C:7]1[CH:11]=[CH:12][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][C:6]=1[OH:13]

参加物

3

反応物 1

HCID 692664-Nitrosalicylic acid

生成物 1

HCID 118160942-Hydroxy-4-nitrobenzyl alcohol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

10.0 g (54.6 mmol) of 4-nitrosalicylic acid are initially charged in 100 ml of THF. With ice-cooling, 109 ml of 1 M borane/THF complex are added, and the mixture is stirred at RT overnight. The mixture is concentrated and the precipitate is filtered off with suction. The solid is dissolved in ethyl acetate and dried over magnesium sulfate. After concentration and drying under high vacuum, the title compound is directly reacted further.

後処理

  1. temperatureWith ice-cooling
  2. addition109 ml of 1 M borane/THF complex are added
  3. concentrationThe mixture is concentrated
  4. filtrationthe precipitate is filtered off with suction
  5. dissolutionThe solid is dissolved in ethyl acetate
  6. dry with materialdried over magnesium sulfate
  7. concentrationAfter concentration
  8. customdrying under high vacuum
  9. customthe title compound is directly reacted further

出典と根拠

ORDレコード
ord-13e21c06ca6a44e48ea17cc79316ba5e
出典データセット
uspto-grants-2010_06
特許番号
US07732477B2

反応ノート

読み込み中…