Reaction equation
[NH:1]([CH2:3][C:4]([O-:6])=[O:5])[CH3:2].[Na+].Cl.[N:9]#[C:10][NH2:11]>>[OH2:5].[O:5]=[C:4]([CH2:3][N:1]([C:10](=[NH:9])[NH2:11])[CH3:2])[OH:6]Participants
Conditions
- Temperature
- 95 °C
Procedure
277.7 g (1 mole) of a technical 40% by weight aqueous sodium sarcosinate solution were used. A pH value of 9.6 (at 20° C.) was adjusted with concentrated hydrochloric acid and heated to 95° C. Subsequently, 105.1 g (1.25 mole) of a technical 50% by weight aqueous cyanamide solution were added thereto with intensive stirring in such a manner that the internal temperature did not exceed 95° C. After ending of the cyanamide addition, further heating was carried out for 1 hour at 95° C. The reaction mixture was then cooled to 15° C. the crystalline precipitate was filtered off with suction and washed chloride-free by washing twice with, in each case, 120 ml of water. The residue was recrystallized from water and dried at 80° C. and 20 mbar. The yield of creatine was 73.4 g (56% of theory). The content determination by means of HPLC gave a content of 100% (creatine monohydrate obtainable pure in chemical commerce was used as standard).
Workup
- customA pH value of 9.6 (at 20° C.)
- customdid not exceed 95° C
- temperaturefurther heating
- temperatureThe reaction mixture was then cooled to 15° C. the crystalline precipitate
- filtrationwas filtered off with suction
- washwashed chloride-free
- washby washing twice with, in each case, 120 ml of water
- customThe residue was recrystallized from water
- customdried at 80° C.
Sources & evidence
- ORD record
- ord-df7ea1d4ddf24e02a917b1f0556d1117
- Source dataset
- uspto-grants-1998_02
- Patent number
- US05719319
Linked notes
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