Water → P-((Acetylamino)methyl)phosphonic acid

HRID 466303

반응식

HRID 466303 반응식
O[CH2:2][NH:3][C:4](=[O:6])[CH3:5].O=P[O:9][P:10]=[O:11].[OH2:12]>C(O)(=O)C>[C:4]([NH:3][CH2:2][P:10]([OH:11])(=[O:12])[OH:9])(=[O:6])[CH3:5]

참가 물질

5

반응물 3

HCID 962WaterHCID 14810Phosphorus trioxideHCID 69365Formicin

생성물 1

HCID 3017080P-((Acetylamino)methyl)phosphonic acid수율 154.4%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
5 °C

실험 절차

20 g (0.225 mol) of N-hydroxymethylacetamide were dissolved in 20 ml of acetic acid and cooled to 5° C. under a nitrogen atmosphere and with stirring. 12.4 g (0.113 mol) of diphosphorus trioxide (P2O3) were then added dropwise at 5° to 10° C. with stirring during the course of 20 minutes. The mixture was then stirred without cooling until room temperature was reached. It was then heated to reflux for 31/2 hours. It was then cooled. 2 g (0.11 mol) of water were then added dropwise with stirring, the temperature rising to 35° C. After cooling, the acetic acid was removed under reduced pressure and with continuous warming to 95° C. The crystalline residue was digested with ethanol. 26 g of crude acetylaminomethanephosphonic acid having a melting point of 171°-175° C. were obtained. After recrystallization from 88% strength aqueous acetic acid, 19 g (55% of theory) of acetylaminomethanephosphonic acid having a melting point of 186° to 90° C. were obtained. The CHNP elemental analysis of a sample gave:

후처리

  1. stirringwith stirring during the course of 20 minutes
  2. stirringThe mixture was then stirred
  3. temperaturewithout cooling until room temperature
  4. temperatureIt was then heated
  5. temperatureto reflux for 31/2 hours
  6. temperatureIt was then cooled
  7. stirringwith stirring
  8. customrising to 35° C
  9. temperatureAfter cooling
  10. customthe acetic acid was removed under reduced pressure
  11. temperaturewith continuous warming to 95° C

출처 및 근거

ORD 기록
ord-967f232b82e44e29ab1118de18402754
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05155257

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