참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 4-Aminobiphenyl | HCID 7102 | — |
| 반응물 | Triethylamine hydrochloride | HCID 11130 | — |
| 반응물 | Phosphorus oxide (P4O10) | HCID 14812 | — |
| 반응물 | Carbonate Ion | HCID 19660 | — |
| 반응물 | 4-(4-Pyridylmethyl)-1(2H)-phtalazinone | HCID 789954 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane methanol | HCID 21226129 | — |
| 생성물 | N-(4-phenylphenyl)-4-(pyridin-4-ylmethyl)phthalazin-1-amine | HCID 6419389 | — |
반응 단계
A mixture of 2.41 g (16.98 mmol) phosphorus pentoxide, 2.32 g (16.85 mmol) triethylamine hydrochloride, 3 g (17.73 mmol) 4-aminobiphenyl, and 1 g (4.21 mmol) 4-(4-pyridylmethyl)-1 (2H)-phthalazinone is stirred for 20 h at 200° C. under a nitrogen atmosphere. After cooling to RT, the hyalinocrystalline melt is distributed between a dichloromethane/methanol mixture (99:1) and a mixture of water and saturated aqueous carbonate solution (1:1) with intensive stirring and the use of an ultrasonic bath. The organic phase dried over sodium sulfate is evaporated under vacuum and the residue purified by means of flash chromatography on silica gel with particle size 0.04-0.06 mm, using a dichloromethane/methanol mixture (49:1). Title compound is obtained after evaporation of the product-containing fractions under vacuum and recrystallization of the residue from acetonitrile; m.p. 189-191° C.; ESI-MS: (M+H)+=389.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06258812B1 |
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| 출처 데이터셋 | uspto-grants-2001_07 |
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| ORD ID | ord-1e62313afc3e418e8c7232f5031a5ced |
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| 출처 메모 | uspto-grants-2001_07 |
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