Hydrochloric Acid → Creatine Monohydrate

HRID 1516964Notes

Reaction equation

HRID 1516964 reaction equation
[NH:1]([CH2:3][C:4]([O-:6])=[O:5])[CH3:2].[Na+].Cl.[N:9]#[C:10][NH2:11]>O>[OH2:5].[O:5]=[C:4]([CH2:3][N:1]([C:10](=[NH:9])[NH2:11])[CH3:2])[OH:6]

Participants

5

Conditions

Temperature
75 °C

Procedure

4625 g (16.7 mol) of a 40% by weight sodium sarcosinate solution prepared according to example 1 was added first. A pH of 9.6 (at 20° C.) was adjusted using concentrated hydrochloric acid while cooling externally with cold water and stirring vigorously. Subsequently it was heated to 75° C. 1403 g (16.7 mol) of a 50% by weight aqueous cyanamide solution (Degussa-Cyanamide L 500) was added uniformly over a period of 90 minutes while stirring vigorously at an internal temperature of 75 to 80° C. After the cyanamide addition was completed, the reaction mixture was stirred for a further 2 hours at an internal temperature of 75° C. After cooling to 5° C., the crystalline reaction product that can be readily filtered was suction filtered, washed three times chloride-free with 1250 ml water in each case and dried in a vacuum-drying cabinet at 40° C. and 20 mbar. The yield was 1897 g creatine monohydrate (corresponds to a yield of 76.2% of theory).

Workup

  1. additionwas added first
  2. customA pH of 9.6 (at 20° C.)
  3. stirringwhile stirring vigorously at an internal temperature of 75 to 80° C
  4. stirringthe reaction mixture was stirred for a further 2 hours at an internal temperature of 75° C
  5. temperatureAfter cooling to 5° C.
  6. filtrationthe crystalline reaction product that can be readily filtered
  7. filtrationfiltered
  8. washwashed three times chloride-free with 1250 ml water in each case
  9. customdried in a vacuum-drying cabinet at 40° C.

Sources & evidence

ORD record
ord-8fc661d9bcad4b2bb722dc5021c98177
Source dataset
uspto-grants-2012_07
Patent number
US08227638B2

Reaction notes

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