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N-Methylaniline → Methyl 4-{[methyl(phenyl)amino]methyl}benzoate

HRID 970824
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 970824
C(OC1C=CC(CO)=CC=1)CC1C=CC=CC=1.[CH3:18][O:19][C:20](=[O:29])[C:21]1[CH:26]=[CH:25][C:24]([CH:27]=O)=[CH:23][CH:22]=1.[CH3:30][NH:31][C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClCCCl>[CH3:18][O:19][C:20](=[O:29])[C:21]1[CH:26]=[CH:25][C:24]([CH2:27][N:31]([CH3:30])[C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)=[CH:23][CH:22]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 7515N-MethylanilineHCID 15294Methyl 4-FormylbenzoateHCID 5049666Sodium triacetoxyborohydrideHCID 12990905(4-Phenethyloxyphenyl)methanol

Produkt 1

HCID 28829589Methyl 4-{[methyl(phenyl)amino]methyl}benzoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 11
1,2-Dichloroethane
Lösungsmittel

Versuchsvorschrift

Following the procedure in J.Org. Chem. 1996, 61 (11), 3849-3862, methyl-4-formylbenzoate (0.821 g, 5.00 mmol) was dissolved in 1,2-dichloroethane (75 ml) at room temperature. N-methylaniline (0.542 ml, 5.00 mmol) was added followed by sodium triacetoxyborohydride (1.484 g, 7.00 mmol). The mixture was allowed to stir at room temperature overnight. The mixture was quenched with saturated sodium bicarbonate solution and extracted with diethyl ether. The organic extracts were dried over anhydrous sodium sulfate and concentrated en vacuo. The residue was purified by-flash chromatography on silica eluted with 4:1 hexane/acetone to give 1.097 g (85.9%) of a slightly yellow oil of 4-[(methyl-phenyl-amino)-methyl]-benzoic acid methyl ester. Reduction to {4-[(methyl-phenyl-amino)-methyl]-phenyl}-methanol, condensation with(R)-2-isocyanato-3-phenyl-propionate of formula 5 and hydrolysis as described for example in Example 1 Steps 2-4, yielded about 1.5 g of 2-{4-[(methyl-phenyl-amino)-methyl]-benzyloxycarbonylamino}-3-phenyl-propionic 169, mp. 69.6-70.1° C.

Aufarbeitung

  1. customThe mixture was quenched with saturated sodium bicarbonate solution
  2. extractionextracted with diethyl ether
  3. dry with materialThe organic extracts were dried over anhydrous sodium sulfate
  4. concentrationconcentrated en vacuo
  5. customThe residue was purified by-flash chromatography on silica
  6. washeluted with 4:1 hexane/acetone

Quellen und Nachweise

ORD-Eintrag
ord-4d55d71cf2584a3abd65aa4b3cbb9ff5
Quelldatensatz
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07312230B2

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