Methanol → 2-Methyl-3-nitrobenzyl alcohol

HRID 476527

반응식

HRID 476527 반응식
[CH3:1][C:2]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][CH:9]=[CH:8][C:3]=1[C:4](OC)=[O:5].[BH4-].[Na+].CO.O>C(O)(C)(C)C>[CH3:1][C:2]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][CH:9]=[CH:8][C:3]=1[CH2:4][OH:5]

참가 물질

6

반응물 4

HCID 887MethanolHCID 962WaterHCID 601165Methyl 2-methyl-3-nitrobenzoateHCID 4311764Sodium borohydride

생성물 1

HCID 902892-Methyl-3-nitrobenzyl alcohol수율 91.8%

시약·촉매·용매 1

HCID 6386tert-Butanol용매

실험 절차

39.0 g (0.2 mol) of methyl 2-methyl-3-nitrobenzoate was dissolved in 600 ml of tert-butanol, and 19.0 g of sodium borohydride was added thereto. Under refluxing, 150 ml of methanol was dropwise added thereto over a period of 1 hour. The refluxing was continued further for 1 hour to complete the reaction. The reaction mixture was left to cool, and then water was added thereto. The solvent was distilled off under reduced pressure. To the residue, water and chloroform were added, and the organic layer was separated and dried over anhydrous sodium sulfate. Then, the solvent was distilled off to obtain 30.7 g of 2-methyl-3-nitrobenzyl alcohol.

후처리

  1. temperatureUnder refluxing
  2. waitThe refluxing was continued further for 1 hour
  3. customthe reaction
  4. waitThe reaction mixture was left
  5. temperatureto cool
  6. distillationThe solvent was distilled off under reduced pressure
  7. additionTo the residue, water and chloroform were added
  8. customthe organic layer was separated
  9. dry with materialdried over anhydrous sodium sulfate
  10. distillationThen, the solvent was distilled off

출처 및 근거

ORD 기록
ord-c8c94b5b103c4b6ea79ec65912403e0d
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04885022

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