Water → 2-Methoxy-6-methylbenzaldehyde

HRID 594283

반응식

HRID 594283 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH3:9])[C:4]=1[CH3:10].C(Cl)Cl.[OH2:14]>CC#N>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH3:9])[C:4]=1[CH:10]=[O:14]

참가 물질

5

반응물 3

HCID 962WaterHCID 6344DichloromethaneHCID 762692,3-Dimethylanisole

생성물 1

HCID 6402382-Methoxy-6-methylbenzaldehyde

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of commercially available 1-methoxy-2,3-dimethylbenzene (10.000 g; 73.40 mmol), copper(II) sulfate pentahydrate CuSO4.5H2O (18.334 g; 73.40 mmol), and potassium peroxodisulfate K2S2O8 (59.547 g; 220.00 mmol) in MeCN (250 ml) and water (250 ml) was heated at reflux, under nitrogen, for 30 min. After cooling to rt, DCM was added and the aq. layer was further extracted with DCM. The mixed organic layers were dried over anh. MgSO4, filtered, and concentrated to dryness under reduced pressure. Purification by FC (heptane/AcOEt=9/1) afforded 2-methoxy-6-methylbenzaldehyde as a yellow oil. LC-MS (conditions A): tR=0.70 min.; no ionisation.

후처리

  1. temperaturewas heated
  2. temperatureat reflux, under nitrogen, for 30 min
  3. extractionthe aq. layer was further extracted with DCM
  4. dry with materialThe mixed organic layers were dried over anh. MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated to dryness under reduced pressure
  7. customPurification by FC (heptane/AcOEt=9/1)

출처 및 근거

ORD 기록
ord-76dc102537034941a646f52f11a5e0eb
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09242970B2

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