Hydrochloric Acid → Creatine Monohydrate

HRID 863207

反応式

HRID 863207 の反応式
[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]

参加物

4

反応条件

温度
95 °C

実験手順

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).

後処理

  1. customA pH value of 9.6 (at 20° C.)
  2. customdid not exceed 95° C
  3. temperaturefurther heating
  4. temperatureThe reaction mixture was then cooled to 15° C. the crystalline precipitate
  5. filtrationwas filtered off with suction
  6. washwashed chloride-free
  7. washby washing twice with, in each case, 120 ml of water
  8. customThe residue was recrystallized from water
  9. customdried at 80° C.

出典と根拠

ORDレコード
ord-df7ea1d4ddf24e02a917b1f0556d1117
出典データセット
uspto-grants-1998_02
特許番号
US05719319

関連ノート

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