참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 4-Sulfophthalic acid | HCID 6962 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 4-Hydroxyphthalic acid | HCID 11881 | 72% |
반응 단계
Sodium hydroxide (251.9 g, 6.30 mol) was added in portions to 4-sulphophthalic acid (50% in water, 258.4 g, 0.525 mol) in a steel vessel accompanied by stirring. After the addition of approx. one third NaOH the increasingly more viscous mixture was heated to 180° C. Once the addition had ended the mixture was stirred for a further 2 h at 200° C. During cooling, the residue was dissolved in water (1000 ml). Conc. hydrochloric acid (620 ml, pH=1) was added accompanied by ice cooling. The solution was extracted with ethyl acetate (5×400 ml). The combined organic phases were dried over Na2SO4, filtered and concentrated on the rotary evaporator. The slightly yellow solid was recrystallized from ethyl acetate. 68.64 g (0.377 mol; 72% yield) of a white solid was obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09393181B2 |
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| 출처 데이터셋 | uspto-grants-2016_07 |
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| ORD ID | ord-e78c004b9e3548b7adb0dc5ce663f69f |
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| 출처 메모 | uspto-grants-2016_07 |
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