Acetic Acid → Creatine

Temperature

15 °C

674.5 g (2.43 moles) of 40% by weight aqueous sodium sarcosinate solution were taken and a pH value of 8.5 adjusted at 70° C. with 99% by weight acetic acid. After the addition of 500 ml methanol, 491.1 g (2.92 moles) of a 25% by weight aqueous cyanamide solution were added thereto with vigorous stirring at reflux temperature in the course of 2 hours. After ending of the addition of the cyanamide solution, the reaction mixture was further stirred for 2 hours under reflux while stirring. After cooling to 15° C., the crystalline precipitate was filtered off with suction, washed twice with, in each case, 250 ml of water and subsequently recrystallised from water. After drying in a vacuum drying cabinet at 80° C. and 15 mbar pressure, there were obtained 176.7 g (48.8% by weight) of anhydrous creatine.

1. additionwere added
2. temperatureat reflux temperature in the course of 2 hours
3. stirringthe reaction mixture was further stirred for 2 hours
4. temperatureunder reflux
5. stirringwhile stirring
6. filtrationthe crystalline precipitate was filtered off with suction
7. washwashed twice with, in each case, 250 ml of water
8. customsubsequently recrystallised from water
9. customAfter drying in a vacuum
10. customdrying cabinet at 80° C.

ORD record

ord-194417aca21c412396fb9f95109f858a

Source dataset

uspto-grants-1998_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05719319