Reaktion #1257666

Reaktionsgleichung

3,4-Methylenedioxyphenethylamine hydrochloride

chloroacetyl chloride

→

N-(2-benzo[1,3]dioxol-5-yl-ethyl)-2-chloro-acetamide

Ausbeute 27.0%

Lösungsmittel

—

TEA

DCE

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenAfter this time, the solution was concentrated down under N2
2. 2
   workup.DISSOLUTIONThe residue was redissolved in DCM
3. 3
   Waschenwashed with sat. NaHCO3 (aq)
4. 4
   Trocknendried over Na2SO4
5. 5
   SonstigeThe crude residue was purified by Prep-LCMS

Vorschrift

3,4-Methylenedioxyphenethylamine hydrochloride (101 mg, 0.5 mmol) was dissolved in DCE (2 mL) and TEA (70 μL). Next, chloroacetyl chloride (48 μL, 0.6 mmol) was added and the reaction was allowed to stir at room temperature for 16 hours. After this time, the solution was concentrated down under N2. The residue was redissolved in DCM, washed with sat. NaHCO3 (aq) and dried over Na2SO4. The crude residue was purified by Prep-LCMS to afford 32 mg (27%) of N-(2-benzo[1,3]dioxol-5-yl-ethyl)-2-chloro-acetamide. 1H-NMR (400 MHz, CDCl3) δ 6.75-6.62 (m, 3H), 5.92 (s, 2H), 4.01 (s, 2H), 3.52-3.47 (m, 2H), 2.79-2.72 (t, 2H).

Quelle