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3-Dimethoxymethyl-4-nitro-benzoic Acid Methyl Ester → 4-Amino-3-dimethoxymethyl-benzoic Acid Methyl Ester

HRID 1788401
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1788401
[CH3:1][O:2][C:3](=[O:18])[C:4]1[CH:9]=[CH:8][C:7]([N+:10]([O-])=O)=[C:6]([CH:13]([O:16][CH3:17])[O:14][CH3:15])[CH:5]=1>CO.[Pd]>[CH3:1][O:2][C:3](=[O:18])[C:4]1[CH:9]=[CH:8][C:7]([NH2:10])=[C:6]([CH:13]([O:14][CH3:15])[O:16][CH3:17])[CH:5]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 1

HCID 576030843-Dimethoxymethyl-4-nitro-benzoic Acid Methyl Ester

Produkt 1

HCID 576031164-Amino-3-dimethoxymethyl-benzoic Acid Methyl Ester

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittel2×

Versuchsvorschrift

100 mg 10% Pd/C and 1 g Mg2SO4 were suspended in 20 mL methanol and were hydrogenated in a Parr apparatus at 30 psi for 15 minutes. The apparatus was opened, and 1.22 g (4.78 mmol) of Compound 5 dissolved in 40 mL methanol was added, followed by 2 mL TEA. The mixture was hydrogenated at 30 psi for 30 minutes, the catalyst was removed by means of filtration and the solution was evaporated to dryness. The solid material was dried over P2O5/H3PO4 overnight to give Compound 6.

Aufarbeitung

  1. additionwas added
  2. waitThe mixture was hydrogenated at 30 psi for 30 minutes
  3. customthe catalyst was removed by means of filtration
  4. customthe solution was evaporated to dryness
  5. dry with materialThe solid material was dried over P2O5/H3PO4 overnight

Quellen und Nachweise

ORD-Eintrag
ord-8abe8252512649bcaa209f9c32202d50
Quelldatensatz
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07511145B2

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