참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Anhydride | HCID 7918 | — |
| 반응물 | Phenylphosphinic acid | HCID 72903 | — |
| 반응물 | N-(hydroxymethyl)benzamide | HCID 80493 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | Phosphinic acid, [(benzoylamino)methyl]phenyl- | HCID 296994 | 73% |
반응 단계
43.2 g (0.424 mol) of acetic anhydride were cooled to 10° C. A solution of 28.2 g (0.2 mol) of benzenephosphonous acid in 40 ml acetic acid were then added dropwise at 15° C., with stirring and cooling. After this, 30.2 g (0.2 mol) of N-hydroxymethylbenzamide were added in portions in the course of 10 minutes at 15° C., with cooling. After this, the cooling was removed, during which process the internal temperature rose to 35° C. After this, the mixture was refluxed for 3 hours and subsequently cooled. 175 ml of water were then added; during this process, the temperature rose to 35° C. The mixture was refluxed again, and finally cooled again, with stirring. After crystallisation, a total of 40 g (73% of theory) of benzoylaminomethylphenylphosphinic acid of a melting point of 158°-160° C. were obtained. CHNP analysis revealed:
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05432291 |
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| 출처 데이터셋 | uspto-grants-1995_07 |
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| ORD ID | ord-6f88232c519d43a2a1bdfc7ba7dae6b1 |
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| 출처 메모 | uspto-grants-1995_07 |
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