참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 1,3-Benzenedimethanamine | HCID 15133 | — |
| 반응물 | 1-[3-Chloro-5-(trifluoromethyl)phenyl]-2,2,2-trifluoroethan-1-one | HCID 53414982 | — |
| 촉매 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | HCID 58247927 | HCID 58247927 | 65.9% |
반응 단계
To a solution of 24.5 g of 1-[3-chloro-5-(trifluoromethyl)phenyl]-2,2,2-trifluoroethanone (88 mmol, 1 eq) in 200 ml of toluene were added 13.6 g of m-(aminomethyl)benzylamine (100 mmol, 1.13 eq). After the addition of a catalytic amount of p-TsOH.H2O (˜100 mg), the mixture was refluxed on a water separator for 12 h (approx. 5 ml of water were removed). Thereafter, another 5.5 g of m-(aminomethyl)benzylamine (40 mmol) were added and the mixture was boiled for a further 11 h. Subsequently, the toluene was distilled off (760 Torr). The resulting crude product was distilled under high vacuum (30-105° C. at 0.5 Ton). Further distillation by means of a Vigreux column (b.p. 105-108° C. at 25 Torr) gives 16.0 g of 1-[3-chloro-5-(trifluoromethyl)phenyl]-2,2,2-trifluoroethanamine (58 mmol, 65%) as a clear liquid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08889878B2 |
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| 출처 데이터셋 | uspto-grants-2014_11 |
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| ORD ID | ord-29fec5e9c9bf4e5eb5957df42af08315 |
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| 출처 메모 | uspto-grants-2014_11 |
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