Acetic Acid → HCID 178511211, 화합물

HRID 278523

반응식

HRID 278523 반응식
C([CH:3]=[CH2:4])=O.C([O:8][C:9](=[O:11])[CH3:10])(=O)C.C[P:13]([O:18]CC)(=O)OCC.[C-]#[N:22].[Na+].[Cl-].[NH4+].Cl.[C:27]([OH:30])(=O)C>N.C(O)C>[NH4+:22].[NH2:22][CH:10]([CH2:4][CH2:3][PH:13]([CH2:27][OH:30])=[O:18])[C:9]([O-:8])=[O:11]

참가 물질

10

반응물 7

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 7847AcroleinHCID 7918Acetic AnhydrideHCID 8929Sodium CyanideHCID 12685Diethyl methylphosphonateHCID 25517Ammonium Chloride

생성물 1

HCID 178511211HCID 178511211, 화합물

시약·촉매·용매 2

HCID 222Ammonia용매HCID 702Ethanol용매

반응 조건

온도
30 °C

실험 절차

At room temperature, 5.61 g (0.10 mol) of freshly distilled acrolein are added to 10.21 g (0.10 mol) of acetic anhydride. At 25-30° C., 13.61 g (0.10 mol) of diethyl methanephosphonate are subsequently added dropwise. The mixture is stirred at 30° C. for 2 hours and then, at 25-28° C., added dropwise to a solution of 4.9 g (0.10 mol) of sodium cyanide and 10.7 g (0.20 mol) of ammonium chloride in 50 ml of ammonia (25% strength). After 2 hours at 30° C., the crude aminonitrile is added dropwise to 200 ml of hydrochloric acid (37% strength). The mixture is subsequently heated under reflux for 2 hours, while ethanol and acetic acid are distilled off. The mixture is concentrated using a rotary evaporator, a pH of approximately 9 is set using ammonia solution and the product is purified by crystallization from methanol. This gives 19.4 g (98% of theory) of 2-amino-4-(hydroxymethylphosphinyl)butyric acid, ammonium salt.

후처리

  1. waitAfter 2 hours at 30° C.
  2. temperatureThe mixture is subsequently heated
  3. distillationare distilled off
  4. concentrationThe mixture is concentrated
  5. customa rotary evaporator
  6. customthe product is purified by crystallization from methanol

출처 및 근거

ORD 기록
ord-22ecc69999914860b72ae2adbe0cf395
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06359162B1

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