반응식
O.[P:2]([OH:5])([OH:4])[OH:3].S(=O)(=O)(O)O.[NH:11]([CH2:16][C:17]([OH:19])=[O:18])[CH2:12][C:13]([OH:15])=[O:14].[CH2:20]=O>>[P:2]([CH2:20][N:11]([CH2:16][C:17]([OH:19])=[O:18])[CH2:12][C:13]([OH:15])=[O:14])([OH:5])([OH:4])=[O:3]참가 물질
반응 조건
- 온도
- 120 °C
실험 절차
Water (17.3 g, 0.961 moles) was charged to a 250 ml three neck flask fitted with thermometer, condenser, dropping funnel and stirrer. Phosphorous acid (42.6 g, 0.514 moles), sulphuric acid (50.0 g, 0.500 moles--added over 10 minutes during which an exotherm from 20° C. to 60° C. was observed) and iminodiacetic acid (66.5 g,0.490 moles) were added to the stirred reaction flask. The reaction mixture was then heated to 120° C. and formaldehyde (48.2 g at 36.1% strength, 0.580 moles) was added over one hour. The temperature was maintained between 110° and 120° C. during addition. On complete addition, the reaction mixture was allowed to cool to 25° C. over 90 minutes and the reaction mixture was filtered. The filter cake was washed with water (57 ml) and the product was dried in a vacuum oven to yield 67.9 g of N-phosphonomethyliminodiacetic acid at 98.0% strength, equivalent to an isolated yield of 59.8%. The filtrates (128.0 g) and the water wash (66.0 g) were analysed at 13.7% and 5.5% N-phosphonomethyliminodiacetic acid respectively. This was equivalent to a total conversion yield of 78.9% N-phosphonomethyliminodiacetic acid.
후처리
- customfitted with thermometer, condenser
- additionwere added to the stirred reaction flask
- temperatureThe temperature was maintained between 110° and 120° C. during addition
- additionOn complete addition
- temperatureto cool to 25° C. over 90 minutes
- filtrationthe reaction mixture was filtered
- washThe filter cake was washed with water (57 ml)
- customthe product was dried in a vacuum oven
출처 및 근거
- ORD 기록
- ord-881c40ec38ba494984efd934042e0713
- 출처 데이터셋
- uspto-grants-1996_06
- 특허 번호
- US05527953
연결된 노트
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