참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | (Aminomethyl)phosphonic acid | HCID 14017 | — |
| 반응물 | 2,4-Dichloro-5-nitrobenzotrifluoride | HCID 621179 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 22132222 | HCID 22132222 | 68.2% |
반응 단계
3.3 g (30 mmol) of aminomethanephosphonic acid in 120 ml of water and 120 ml of ethanol are introduced together with 3.37 g (31.8 mmol) of soda and mixed with 7.8 g (97%, 30 mmol) of 3-trifluoromethyl-4,6-dichloronitrobenzene, and it is refluxed for 4 hours at 120° C. bath temperature. After removing the ethanol in a rotary evaporator, it is extracted three times with 100 ml of ethyl acetate. The organic phase is washed with a little water. It contains starting material and is discarded. The collected aqueous phase is adjusted acidic with 4 N hydrochloric acid to pH 1 and extracted three times with 100 ml of ethyl acetate each. The organic phase is washed with water, dried, filtered and concentrated by evaporation. 6.85 g (68% of theory) of N-(2-nitro-4-trifluoromethyl-5-chloro-phenyl)-aminomethanephosphonic acid of melting point 207.3° C. is obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05955461 |
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| 출처 데이터셋 | uspto-grants-1999_09 |
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| ORD ID | ord-59297c84265743d68a9221d0db48b81b |
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| 출처 메모 | uspto-grants-1999_09 |
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