2-Methyl-5-nitrobenzoic acid → (2-Methyl-5-nitrophenyl)methanol

HRID 1946343

반응식

HRID 1946343 반응식
[CH3:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4](O)=[O:5]>C1COCC1.CO>[CH3:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[CH2:4][OH:5]

참가 물질

4

반응물 1

HCID 5196832-Methyl-5-nitrobenzoic acid

생성물 1

HCID 3567085(2-Methyl-5-nitrophenyl)methanol수율 114.6%

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 8028Tetrahydrofuran용매

반응 조건

온도
80 °C

실험 절차

To a solution of 2-methyl-5-nitrobenzoic acid (3.0 g, 16.6 mmol, Acros) in THF (60 ml) at ambient temperature under nitrogen was added dropwise 1.0 M borane-tetrahydrofuran complex (33.1 ml, 33.1 mmol, Aldrich). The solution was heated to 80° C. for 1.5 h. To the solution at ambient temperature was slowly added methanol (20 ml) and then heated to 80° C. for 30 min. The solvent was removed in vacuo to leave an oil. The residue was dissolved in methanol (approximately 30 ml) and the solvent removed in vacuo to give (2-methyl-5-nitrophenyl)methanol as a yellow solid (3.18 g).

후처리

  1. customat ambient temperature
  2. temperatureheated to 80° C. for 30 min
  3. customThe solvent was removed in vacuo
  4. customto leave an oil
  5. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-a27c82ea6a4045009aa1b2b79a3bb9cd
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08399436B2

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