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

HRID 335572

반응식

HRID 335572 반응식
[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]

참가 물질

3

반응물 1

HCID 692664-Nitrosalicylic acid

생성물 1

HCID 118160942-Hydroxy-4-nitrobenzyl alcohol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-233a740a673244c8a19524f936c63ad0
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08884017B2

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