Hydrochloric Acid → Glyphosate

HRID 279799

반응식

HRID 279799 반응식
[N:1]1([CH2:7][P:8](=[O:11])([OH:10])[OH:9])[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[OH-:12].[Na+].Cl>O>[P:8]([CH2:7][NH:1][CH2:6][C:5]([OH:12])=[O:4])([OH:9])([OH:10])=[O:11].[NH2:1][CH2:7][P:8](=[O:9])([OH:11])[OH:10].[OH:4][CH2:3][CH2:2][NH:1][CH2:7][P:8](=[O:9])([OH:11])[OH:10]

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 4491459Morpholinomethylphosphonic acid

생성물 3

HCID 3496Glyphosate수율 34.7%HCID 14017(Aminomethyl)phosphonic acid수율 23%HCID 10942688N-(2-hydroxyethyl)aminomethylphosphonic acid수율 19.6%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
275 °C

실험 절차

In a 100 mL Monel autoclave were mixed 4.0 g (22 mmol) of 4-morpholinylmethylphosphonic acid and 26.3 g (330 mmol) of a 50.3% solution of NaOH. The vessel was sealed and heated to 275° C. for four hours. The reaction was cooled to room temperature and the residual pressure generated by the reaction was vented off. The reaction mixture was a white slurry which was diluted with 10 mL of H2O and neutralized with 27.2 mL (330 mmol) of conc. HCl. This solution was concentrated to dryness. The residue was taken up in conc. HCl and the precipitated NaCl was filtered off. The filtrate was concentrated and purified by ion exchange chromatography to yield 1.29 g (34.7%) of N-phosphonomethylglycine, 0.57 g (23%) of aminomethylphosphonic acid, 0.67 g (19.6%) of N-(2-hydroxyethyl)aminomethylphosphonic acid, and 0.46 g (11.6%) of unreacted starting material.

후처리

  1. customThe vessel was sealed
  2. temperatureThe reaction was cooled to room temperature
  3. concentrationThis solution was concentrated to dryness
  4. filtrationthe precipitated NaCl was filtered off
  5. concentrationThe filtrate was concentrated
  6. custompurified by ion exchange chromatography

출처 및 근거

ORD 기록
ord-cfea267b03ce4365b5c51e32b62eb2d8
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04587061

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