Water → 2-Methoxy-6-methylbenzaldehyde

HRID 594283

反応式

HRID 594283 の反応式
[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]

参加物

5

反応物 3

HCID 962WaterHCID 6344DichloromethaneHCID 762692,3-Dimethylanisole

生成物 1

HCID 6402382-Methoxy-6-methylbenzaldehyde

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-76dc102537034941a646f52f11a5e0eb
出典データセット
uspto-grants-2016_01
特許番号
US09242970B2

関連ノート

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