참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Heptane | HCID 8900 | — |
| 반응물 | 2-Chloro-4,6-diphenyl-1,3,5-triazine | HCID 19698 | — |
| 반응물 | N-Phenyl-o-phenylenediamine | HCID 68297 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 58399779 | HCID 58399779 | 88% |
반응 단계
44.3 g (240 mmol) of N-phenyl-o-phenylenediamine are initially introduced in THF and cooled to 0° C., and 136.4 ml (818 mmol) of N-ethyldiisopropylamine are added dropwise. The mixture is subsequently stirred at room temperature for a further 1 h. A solution of 64.4 g (240 mmol) of 2-chloro-4,6-diphenyl-1,3,5-triazine, dissolved in 1600 ml of THF, is then added dropwise, and the mixture is stirred at 60° C. for 96 h. After cooling, the solution is stirred with 400 ml of heptane, 80 ml of dichloromethane and 100 ml of ethanol. The solid is washed with toluene and washed by stirring with hot heptane, giving 87.7 g (211 mmol) of a crystalline solid. The overall yield is 88%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08865321B2 |
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| 출처 데이터셋 | uspto-grants-2014_10 |
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| ORD ID | ord-7e95338f771b4a278185053804772dc4 |
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| 출처 메모 | uspto-grants-2014_10 |
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