Reaktion #67487

ord-1b3390e9bfa64341bea863de1043ac68

Reaktionsgleichung

CN(C)[C@@H](CC(=O)O)C(=O)O
dimethylaspartic acid
O=S(=O)(O)O
sulfuric acid
→
CN(C)[C@@H](CC(=O)O)C(=O)O.O=S(=O)(O)O
N,N-dimethylaspartic acid sulfate
Ausbeute 95.4%

Edukte

CN(C)[C@@H](CC(=O)O)C(=O)O
dimethylaspartic acid
O=S(=O)(O)O
sulfuric acid

Reagenzien

Keine

Lösungsmittel

O
water

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONAfter the addition
  2. 2
    workup.WAITa reaction was conducted for 2 hours
  3. 3
    EinengenThe reaction solution was concentrated
  4. 4
    Sonstigeazeotroped with 100 ml of toluene
  5. 5
    Sonstigeto further remove the water
  6. 6
    SonstigeAfterwards, the product was dried under high vacuum, and ground

Vorschrift

10 g of dimethylaspartic acid was placed in a 250 ml round-bottom flask, and 40 ml of water was added and stirred for 30 minutes. Then, 7.36 g of concentrated sulfuric acid (concentration: 98%) was slowly added to the flask. After the addition, a reaction was conducted for 2 hours. The reaction solution was concentrated, and azeotroped with 100 ml of toluene to further remove the water. Afterwards, the product was dried under high vacuum, and ground by using a spatula to obtain 15.34 g of N,N-dimethylaspartic acid sulfate as tawny oil (Yield: 95.33%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524895B2uspto-grants-2013_09