Sodium Chloride → Methyl (3-bromobenzyl)carbamate

HRID 427250Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 427250
Cl.[Br:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH2:6][NH2:7].C(N(CC)CC)C.Cl[C:19]([O:21][CH3:22])=[O:20].[Cl-].[Na+]>C(Cl)(Cl)Cl>[Br:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH2:6][NH:7][C:19](=[O:20])[O:21][CH3:22]

Komponenten

6

Edukt 4

HCID 5234Sodium ChlorideHCID 6586Methyl chloroformateHCID 8471TriethylamineHCID 27249803-Bromobenzylamine hydrochloride

Produkt 1

HCID 12090302Methyl (3-bromobenzyl)carbamateAusbeute 87 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

To a suspension of 10.0 g of 3-bromobenzylamine hydrochloride in chloroform (100 ml), 9.55 g of triethylamine was added at room temperature. To this solution, 4.67 g of methyl chloroformate was dropwise added under cooling with ice, followed by stirring at room temperature for 2 hours. The reaction solution was poured into a sodium chloride aqueous solution, and the organic layer was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography to obtain 9.54 g of methyl N-(3-bromobenzyl)carbamate as white crystals.

Aufarbeitung

  1. additionwas added at room temperature
  2. temperatureunder cooling with ice
  3. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  4. distillationThe solvent was distilled off under reduced pressure
  5. customthe residue was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-2e7b3b0e1e124827b5f8cf77d7fe0b6a
Quelldatensatz
uspto-grants-2001_11
Patentnummer
US06313071B1

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