Pyridine → 3-(2-Methoxyphenyl)propionamide

HRID 480703

Reaktionsgleichung

Reaktionsgleichung von HRID 480703
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:9][CH2:10][C:11]([OH:13])=O.[N:14]1C=CC=CC=1.C(OC(OC(C)(C)C)=O)(OC(C)(C)C)=O.C(=O)([O-])O.[NH4+]>C(#N)C>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:9][CH2:10][C:11]([NH2:14])=[O:13]

Komponenten

6

Versuchsvorschrift

3-(2-methoxyphenyl)propionic acid (9.0 g, 49.9 mmol) was dissolved in acetonitrile (10 mL). Subsequently, pyridine (3.54 g, 44.9 mmol) and di-tert-butyl dicarbonate [Boc2O (16.3 g, 74.85 mmol)] were added thereto. The mixture was stirred for 10 minutes at room temperature, and then ammonium hydrogencarbonate (5.92 g, 74.9 mmol) were added. After completion of reaction, the reaction mixture was concentrated under reduced pressure. Thereafter, the resultant concentrate was added to water, and the resultant mixture was extracted with chloroform, followed by washing sequentially with 1M hydrochloric acid and saturated brine. The resultant mixture was subjected to drying over magnesium sulfate and concentration under reduced pressure. The resultant concentrate was used in Production Example 36 without purification.

Aufarbeitung

  1. customAfter completion of reaction
  2. concentrationthe reaction mixture was concentrated under reduced pressure
  3. concentrationThereafter, the resultant concentrate
  4. additionwas added to water
  5. extractionthe resultant mixture was extracted with chloroform
  6. washby washing sequentially with 1M hydrochloric acid and saturated brine
  7. dry with materialto drying over magnesium sulfate and concentration under reduced pressure
  8. concentrationThe resultant concentrate
  9. customwas used in Production Example 36 without purification

Quellen und Nachweise

ORD-Eintrag
ord-f1e930a46d5e40c7b88bebef76659de2
Quelldatensatz
uspto-grants-2003_11
Patentnummer
US06653334B1

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