Réaction #75985

ord-417ec7c912ae449591fed87b6ab6f8ba

Conditions de réaction

Température
100°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    workup.DISSOLUTIONthe suspension dissolves when hot
  2. 2
    TempératureThe reaction mixture is then cooled to a temperature in the region of 0° C.
  3. 3
    Filtrationfinally filtered through a sinter funnel
  4. 4
    LavageThe filter cake is washed with twice 50 cm3 of filtrate
  5. 5
    Autredried in a fume cupboard
  6. 6
    Autrein the region of 60° C

Mode opératoire

A suspension of 34 g of diethyl 2-(acetylamino)-2-(3-nitrobenzyl)malonate in 510 cm3 of concentrated hydrochloric acid is heated at a temperature in the region of 100° C. for 18 hours: a vigorous evolution of gas takes place and the suspension dissolves when hot. The reaction mixture is then cooled to a temperature in the region of 0° C., after which it is stirred for 1 hour at 0° C. and finally filtered through a sinter funnel. The filter cake is washed with twice 50 cm3 of filtrate and dried in a fume cupboard and then in an oven under vacuum (10 Pa) at a temperature in the region of 60° C. 23.4 g of 3-nitrophenylalanine hydrochloride are obtained in the form of white crystals melting at 222° C.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US06699895B2uspto-grants-2004_03