Reaktion #93066

ord-80bd70f61956487b962e5c35298033de

Reaktionsgleichung

CC(C)CC(N)C(=O)O
DL-leucine
O=C(O)C[C@H](NC(=O)OCc1ccccc1)C(=O)O
N-carbobenzoxy-L-aspartic acid
O=S(=O)(O)O
sulfuric acid
→
CC(C)C[C@H](N)C(=O)O.O=C(O)C[C@H](NC(=O)OCc1ccccc1)C(=O)O
L-leucine N-carbobenzoxy-L-aspartic acid
Ausbeute 50.0%

Edukte

CC(C)CC(N)C(=O)O
DL-leucine
O=C(O)C[C@H](NC(=O)OCc1ccccc1)C(=O)O
N-carbobenzoxy-L-aspartic acid
O=S(=O)(O)O
sulfuric acid

Reagenzien

Keine

Lösungsmittel

O
water

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThis solution was cooled to 10° C. at a rate of 2° C. per hour
  2. 2
    workup.STIRRINGwas stirred for another two hours
  3. 3
    SonstigeThe resulting crystal was separated
  4. 4
    Waschenwashed with 30 ml of water
  5. 5
    Sonstigedried

Vorschrift

Ten grams of DL-leucine, 12.2 g of N-carbobenzoxy-L-aspartic acid and 1.9 g of sulfuric acid were added to 500 ml of water and the resulting solution was heated to 60° C. This solution was cooled to 10° C. at a rate of 2° C. per hour while stirring, and was stirred for another two hours. The resulting crystal was separated, washed with 30 ml of water and dried to give 9.1 g of an L-leucine/N-carbobenzoxy-L-aspartic acid. Analysis showed that the optical purity of the L-leucine was 95%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04610827uspto-grants-1986_09