Hydrochloric Acid → Glyphosate

HRID 279799

反応式

HRID 279799 の反応式
[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]

参加物

7

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 4491459Morpholinomethylphosphonic acid

生成物 3

HCID 3496Glyphosate収率 34.7%HCID 14017(Aminomethyl)phosphonic acid収率 23%HCID 10942688N-(2-hydroxyethyl)aminomethylphosphonic acid収率 19.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
275 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-cfea267b03ce4365b5c51e32b62eb2d8
出典データセット
uspto-grants-1986_05
特許番号
US04587061

関連ノート

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