Acetic Acid → Creatine

HRID 863209

반응식

HRID 863209 반응식
[NH:1]([CH2:3][C:4]([O-:6])=[O:5])[CH3:2].[Na+].C(O)(=O)C.[N:12]#[C:13][NH2:14]>CO>[O:5]=[C:4]([CH2:3][N:1]([C:13](=[NH:12])[NH2:14])[CH3:2])[OH:6]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 9864Cyanamide2회HCID 23667259Sodium Sarcosinate

생성물 1

HCID 586Creatine

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
15 °C

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-194417aca21c412396fb9f95109f858a
출처 데이터셋
uspto-grants-1998_02
특허 번호
US05719319

연결된 노트

불러오는 중…