Methanol → 3-(methoxymethyl)benzoic Acid

HRID 980462노트

반응식

HRID 980462 반응식
Br[CH2:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6]([OH:8])=[O:7].[CH3:12][OH:13]>C[O-].[Na+]>[CH3:12][O:13][CH2:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6]([OH:8])=[O:7]

참가 물질

4

반응물 2

HCID 887MethanolHCID 2456503-(Bromomethyl)benzoic acid

생성물 1

HCID 49623543-(methoxymethyl)benzoic Acid수율 92%

시약·촉매·용매 1

HCID 10942334Sodium Methoxide용매

실험 절차

12 g (55.75 millimoles) of 3-bromomethyl-benzoic acid are dissolved in 10 ml of anhydrous methanol and to the solution 22.30 ml of sodium methylate (concentration 5 millimoles/ml) are added dropwise at room temperature. The reaction mixture is stirred for 5-10 minutes, the methanol is removed in vacuo. The residue is dissolved in 10 ml of ethyl acetate, to the solution 2 ml of water are added and the pH of the mixture is adjusted to 2-3 with a 2N sodium hydrogen sulfate solution at 0° C. The layers are separated, the organic phase is dried, filtered and the solvent is distilled off in vacuo. Thus 8.55 g of the title compound are obtained, yield 92,3%.

후처리

  1. additionare added dropwise at room temperature
  2. customthe methanol is removed in vacuo
  3. dissolutionThe residue is dissolved in 10 ml of ethyl acetate, to the solution 2 ml of water
  4. additionare added
  5. customis adjusted to 2-3 with a 2N sodium hydrogen sulfate solution at 0° C
  6. customThe layers are separated
  7. customthe organic phase is dried
  8. filtrationfiltered
  9. distillationthe solvent is distilled off in vacuo

출처 및 근거

ORD 기록
ord-adc8b7794f1e4a2488898ebc3ce61137
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04638002

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