Réaction #67487

ord-1b3390e9bfa64341bea863de1043ac68

Équation de réaction

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
Rendement 95.4%

Réactifs

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

Réactifs

Aucun

Solvants

O
water

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

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

Mode opératoire

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%).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08524895B2uspto-grants-2013_09