Reaktion #1563910

ord-46185baa8e6f4595a312b450072fd88c

Reaktionsgleichung

[Na+].[OH-]
NaOH
NCc1ccc2c(c1)OCO2
3,4-methylenedioxybenzylamine
CC(=O)OC(C)=O
acetic anhydride
CC(=O)NCc1ccc2c(c1)OCO2
N-(benzo[d][1,3]dioxol-5-ylmethyl)acetamide
Ausbeute 77.0%

Lösungsmittel

Reaktionsbedingungen

Temperatur
20°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe mixture was filtered
  2. 2
    Sonstigeto obtain a solid which
  3. 3
    Waschenwas washed water
  4. 4
    Sonstigedried in vacuum

Vorschrift

To a solution of 3,4-methylenedioxybenzylamine (10 g, 66.2 mmol) in acetic acid (50 mL) was added acetic anhydride (15.27 g, 150 mmol). The mixture was stirred at 20° C. for 30 minutes. Then it was adjusted to PH7 with 10% NaOH. The mixture was filtered to obtain a solid which was washed water and dried in vacuum to give N-(benzo[d][1,3]dioxol-5-ylmethyl)acetamide as a white solid (9.24 g, 77%). LC-MS: 194 [M+1]+; 1H-NMR (DMSO-d6): δ 1.84 (s, 3H), 4.12 (d, 2H, J=6.4 Hz), 5.98 (s, 2H), 6.71 (m, 2H), 6.83 (m, 2H), 8.28 (s, 1H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09402832B2uspto-grants-2016_08