참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 1,2,4-Trimethylbenzene | HCID 7247 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 3-Trifluoropropylamino-4-methylphenol | HCID 54349738 | — |
| 생성물 | HCID 178421808 | HCID 178421808 | — |
반응 단계
The pseudocumene layer from alkylation, containing 0.35-0.38 mole of 3-trifluoropropylamino-4-methylphenol was refluxed in a 1 L 3-necked flask fitted with thermometer, stirrer and Dean-Stark trap in order to remove water as the azeotrope. To the dry solution was added 30 g of phthalic anhydride. Condensation was effected by heating at reflux for 20 hours while removing water generated by reaction as the pseudocumene-water azeotrope. The solution turned red. When condensation was complete the solution was cooled to 100° C., 300 ml water and 25 g 50% sodium hydroxide added, and the pseudocumene removed by azeotropic distillation. The red dye which had crystallized out was separated by filtration and washed with 400 ml water (142 g wet paste). This filtercake was reslurried in 400 ml water and 10 g 50% sodium hydroxide, heated 30 minutes at 100° C., filtered again and washed with 400 ml water. Upon drying at 100° C., 40 g of dye zwitterion was obtained which melted at 258°-260° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05047559 |
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| 출처 데이터셋 | uspto-grants-1991_09 |
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| ORD ID | ord-7f31f22035324278a49305eb62f7d50f |
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| 출처 메모 | uspto-grants-1991_09 |
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