Sodium Chloride → HCID 12090302, Verbindung

HRID 1168035Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1168035
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 12090302HCID 12090302, VerbindungAusbeute 87 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

10.00 g of 3-bromobenzylamine hydrochloride suspended in chloroform (100 ml) was mixed with 9.55 g of triethylamine at room temperature. The resulting solution was stirred under cooling with ice while 4.67 g of methyl chloroformate was added dropwise and then stirred at room temperature for 2 hours. After the reaction, the reaction solution was poured into saturated aqueous sodium chloride, and the organic layer was separated, dried over anhydrous magnesium sulfate and evaporated at ordinary pressure for removal of the solvent. The residue was purified by silica gel column chromatography to give 9.54 g of methyl N-(3-bromobenzyl)carbamate as white crystals. m.p. 41-44° C.

Aufarbeitung

  1. additionwas added dropwise
  2. stirringstirred at room temperature for 2 hours
  3. customAfter the reaction
  4. customthe organic layer was separated
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated at ordinary pressure for removal of the solvent
  7. customThe residue was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-843bda6c90424b4391826737afe549f1
Quelldatensatz
uspto-grants-2003_09
Patentnummer
US06620961B1

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