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Acetic Acid → (5-Bromo-2-iodo-benzyl)-ethyl-amine

HRID 1625672
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1625672
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([I:10])=[C:6]([CH:9]=1)[CH:7]=O.[CH2:11]([NH2:13])[CH3:12].C(O)(=O)C.C([BH3-])#N.[Na+]>CO>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([I:10])=[C:6]([CH:9]=1)[CH2:7][NH:13][CH2:11][CH3:12]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 176Acetic AcidHCID 6341EthylamineHCID 5003444Sodium cyanoborohydrideHCID 219738615-Bromo-2-iodobenzaldehyde

Produkt 1

HCID 58148919(5-Bromo-2-iodo-benzyl)-ethyl-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To 5-bromo-2-iodo-benzaldehyde (15.0 g, 48.3 mmol) in methanol (60 mL) was added ethylamine (2.0M in methanol; 48 mL, 72.0 mmol), followed by acetic acid (3.0 mL, 53.4 mmol), and the mixture was stirred at room temperature for 30 minutes, after which a precipitate formed. Sodium cyanoborohydride (6.00 g, 95.4 mmol) was then added in 3 portions and the precipitate disappeared. The reaction was stirred at room temperature for 24 hours then quenched with saturated aqueous sodium bicarbonate. The resulting mixture was evaporated then diluted with dichloromethane and washed with water, dried over magnesium sulfate, filtered, and concentrated. The residue was purified by silica gel chromatography (0-4% methanol in dichloromethane) to give the title compound.

Aufarbeitung

  1. customafter which a precipitate formed
  2. stirringThe reaction was stirred at room temperature for 24 hours
  3. customthen quenched with saturated aqueous sodium bicarbonate
  4. customThe resulting mixture was evaporated
  5. additionthen diluted with dichloromethane
  6. washwashed with water
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customThe residue was purified by silica gel chromatography (0-4% methanol in dichloromethane)

Quellen und Nachweise

ORD-Eintrag
ord-5f82fe486a71488e898637325541a050
Quelldatensatz
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08785393B2

Notizen zur Reaktion

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