참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | Triclosan | HCID 5564 | — |
| 반응물 | Thionyl Chloride | HCID 24386 | — |
| 반응물 | 2-Hexadecanoyloxy-1-(hexadecanoyloxymethyl)ethyl hydrogen glutarate | HCID 23322903 | — |
| 용매 | Cyclohexane | HCID 8078 | — |
| 생성물 | HCID 54422056 | HCID 54422056 | — |
반응 단계
A mixture of cyclohexane (60 ml.), pyridine (1.43 ml.) and 2-hexadecanoyloxy-1-(hexadecanoyloxymethyl)ethyl hydrogen glutarate (B) (11.0 g.) was warmed to 35° C. The solution obtained was added dropwise during 45 minutes to a stirred solution of thionyl chloride (1.23 ml.) in cyclohexane (25 ml.) at 35° C. The mixture was then stirred for a further 1.5 hours at 35° C., cooled to 15° C. and a solution of triclosan (4.68 g.) and pyridine (1.56 ml.) in cyclohexane (20 ml.) added during 15 minutes. The mixture was stirred at ambient temperature for 16 hours, warmed to 35° C. and washed first with 0.5 M hydrochloric acid (100 ml.) and then with water (3×100 ml.), also heated to 35° C. The mixture was then dried (MgSO4) and evaporated to give 5-chloro-2-(2,4-dichlorophenoxy)phenyl 2-hexadecanoyloxy-1-(hexadecanoyloxymethyl)ethyl glutarate as a white solid, m.p. 44°-46° C., identical with the material obtained in Example 4 as judged by its NMR and mass spectral properties.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04587262 |
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| 출처 데이터셋 | uspto-grants-1986_05 |
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| ORD ID | ord-b9c7435022e044fba33b4ced42b2f2cc |
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| 출처 메모 | uspto-grants-1986_05 |
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