참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Propylamine | HCID 7852 | — |
| 반응물 | 1,3,5-Trichloro-2-(2-chloroethoxy)benzene | HCID 11276959 | — |
| 생성물 | N-(2-(2,4,6-Trichlorophenoxy)ethyl)-1-propanamine | HCID 3842173 | 93% |
반응 단계
Into a 1-liter glass reactor, which could withstand a pressure of 6 atmospheres, fitted with a stirrer, heating mantle and a pressure gauge, were added 270.8 g 2-(2,4,6-trichlorophenoxy) ethyl chloride and 350 g n-propyl amine. The mixture was slowly heated with stirring over a period of 8 hours at a temperature of 90° C. The initial pressure under these conditions was 3 atmospheres, which dropped during the reaction to about 2.2 atmospheres. The end of the reaction was determined by GLC. At the end of the reaction the mixture was cooled to 55° C., whereupon the pressure dropped to atmospheric. The excess n-propyl amine was distilled off and it could be recycled for use in a subsequent batch, until a bottom temperature of 85° C. was reached. At the end of the distillation the mixture was cooled to 40° C., 300 ml of a 20% hydrogen chloride solution and 1 g of an emulgator GAF RM-510 were added. The temperature rose to 70° C., the mixture was stirred for one hour at this temperature and the product precipitated as white crystals of the amine hydrochloride salt. The slurry is cooled to 40° C., filtered, re-slurried in 250 ml xylene and filtered again. This affords 312 g of white hydrochloride salt of N-n-propyl-N-2-(2,4,6-trichlorophenoxy)-ethyl amine in 93% yield and purity of 96%-98%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05091578 |
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| 출처 데이터셋 | uspto-grants-1992_02 |
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| ORD ID | ord-9a3243feb82a422eaa2d8b4a536eeff9 |
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| 출처 메모 | uspto-grants-1992_02 |
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