Sulfuric Acid → N-methylaspartic acid sulfate

HRID 39211Notes

Reaction equation

HRID 39211 reaction equation
[CH3:1][NH:2][C@H:3]([C:8]([OH:10])=[O:9])[CH2:4][C:5]([OH:7])=[O:6].[S:11](=[O:15])(=[O:14])([OH:13])[OH:12]>O>[S:11]([OH:15])([OH:14])(=[O:13])=[O:12].[CH3:1][NH:2][C@H:3]([C:8]([OH:10])=[O:9])[CH2:4][C:5]([OH:7])=[O:6]

Participants

4

Reactant 2

HCID 1118Sulfuric AcidHCID 92982N-Methyl-L-aspartic acid

Product 1

HCID 86639894N-methylaspartic acid sulfateYield 95.5%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

10.7 g of N-methylaspartic acid was placed in a 250 ml round-bottom flask, and 100 ml of water was added to the flask and stirred for 30 minutes by using a magnetic stirrer. 7.12 g of concentrate sulfuric acid (concentration: 98%) was slowly dropped into the flask under stirring, and stirred for additional 2 hours after dropping. After the reaction, the reaction solution was concentrated, azeotroped with 100 ml of toluene to further remove the water and dried under vacuum to obtain 17 g of N-methylaspartic acid sulfate as yellow oil (Yield: 95.3%).

Workup

  1. stirringunder stirring
  2. stirringstirred for additional 2 hours
  3. customAfter the reaction
  4. concentrationthe reaction solution was concentrated
  5. customazeotroped with 100 ml of toluene
  6. customto further remove the water
  7. customdried under vacuum

Sources & evidence

ORD record
ord-53db3abe415442db8d58a89781f64b4c
Source dataset
uspto-grants-2013_09
Patent number
US08524895B2

Reaction notes

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