참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | O-Xylene | HCID 7237 | — |
| 반응물 | 4-Methylpentane-1,2-diol | HCID 91171 | — |
| 반응물 | Potassium Fluoride | HCID 522689 | — |
| 반응물 | 2,4-Dichloro-5-fluorobenzonitrile | HCID 2782753 | — |
| 촉매 | Tetrabutylphosphonium bromide | HCID 76564 | — |
| 생성물 | 2-Chloro-4,5-difluorobenzonitrile | HCID 4085849 | — |
반응 단계
In a 100 ml flange flask fitted with a distillation bridge and anchor stirrer, 14.5 g (0.25 mol) of potassium fluoride, 4.8 g (0.007 mol) of trimethyl(ethoxypolyoxypropyl)ammonium chloride, 6.2 g (0.012 mol) of polyethylene glycol dimethyl ether 500 and 2.4 g (0.007 mol) of tetrabutylphosphonium bromide were introduced at 100° C. into the melt of 47.5 g (0.25 mol) of 2,4-dichloro-5-fluorobenzonitrile. Subsequently, 10 g (0.09 mol) of xylene were added and the reaction suspension was azeotropically dried by application of a vacuum of 20 mbar and heating to 130° C. After the xylene had been distilled off, the reaction suspension was heated to 140° C. and stirred for 8 hours at this temperature. Amount of 2-chloro-4,5-difluorobenzonitrile formed:
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05466859 |
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| 출처 데이터셋 | uspto-grants-1995_11 |
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| ORD ID | ord-6f0eb02cbc95451ca753776a47119975 |
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| 출처 메모 | uspto-grants-1995_11 |
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