참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrazine | HCID 9321 | — |
| 반응물 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 반응물 | 2,2-Bis(3-nitro-4-hydroxyphenyl)hexafluoropropane | HCID 11133683 | — |
| 촉매 | Nickel | HCID 935 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 2,2-Bis(3-amino-4-hydroxyphenyl)hexafluoropropane | HCID 632603 | — |
반응 단계
100.0 g of 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane, 300 cc of methanol, and 5.0 g of developed NDT-90 (trade name, Raney nickel catalyst, manufactured by Kawaken Fine Chemical Co.) were put into a 500-cc four-neck flask equipped with a thermometer, a Dimroth condenser and a stirrer, and heated, with stirring, up to 60° C. to completely dissolve 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane in the solvent. The resulting solution was kept at 60 to 65° C., to which was dropwise added 78.3 g of an aqueous solution of 60% hydrazine monohydrate over a period of 1 hour. After the aqueous hydrazine solution was added, the mixture was stirred for further 30 minutes, and then gradually cooled to room temperature. After the catalyst was removed through filtration, the reaction mixture was concentrated to obtain a crude product of 2,2-bis(3-amino-4-hydroxy-phenyl)hexafluoropropane. The crude yield was 82.5 g (96.0%). The purity in liquid chromatography was 96.5% (area %).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05977413 |
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| 출처 데이터셋 | uspto-grants-1999_11 |
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| ORD ID | ord-752f8180d40f45c19eea3de3e1ee3426 |
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| 출처 메모 | uspto-grants-1999_11 |
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