Reaktion #743614

ord-0dd147242d854f14bb7efe4abc9e2405

Reaktionsgleichung

CC(C)(C)c1ccc2c(c1)CCC2N
5-tert-Butyl-2,3-dihydro-1H-inden-1-ylamine
CC(=O)N[C@@H](CC(C)C)C(=O)O
N-acetyl-(L)-leucine
CC(C)(C)c1ccc2c(c1)CC[C@@H]2N
title compound
CC(C)(C)c1ccc2c(c1)CC[C@@H]2N
(1S)-5-tert-butyl-2,3-dihydro-1H-inden-1-ylamine

Lösungsmittel

Reaktionsbedingungen

Temperatur
65°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto cool to ambient temperature
  2. 2
    FiltrationThe solids were filtered
  3. 3
    Waschenwashed with toluene
  4. 4
    Temperaturto reflux
  5. 5
    Temperaturto cool to ambient temperature
  6. 6
    Filtrationthe solids were filtered
  7. 7
    SonstigeThe solid was dried at 40° C. under reduced pressure

Vorschrift

5-tert-Butyl-2,3-dihydro-1H-inden-1-ylamine (25.51 g, 93% potency), N-acetyl-(L)-leucine (23.34 g), and methanol (315 mL) were combined and heated at 65° C. for 1 hour. The solution was allowed to cool to ambient temperature. The solids were filtered and washed with toluene. The solid was then resuspended in methanol (125 mL) and brought to reflux. The solution was allowed to cool to ambient temperature and the solids were filtered. The solid was dried at 40° C. under reduced pressure to provide the title compound (98.7% ee).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08071762B2uspto-grants-2011_12