참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Benzene | HCID 241 | — |
| 반응물 | p-Toluenesulfonic acid | HCID 6101 | — |
| 반응물 | 1-Dodecanol | HCID 8193 | — |
| 반응물 | 2-Chloro-3-hydroxypropionic acid | HCID 564951 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 86651356 | HCID 86651356 | — |
반응 단계
2-chloro-3-hydroxypropionic acid (4.80 g, 0.03 mol), dodecanol (6.00 g, 0.03 mol) were taken with 5 mL dry benzene in a (50 mL) RB, with a dean-stark apparatus and condenser; 25 mg (0.26 mmol) para-Toluene sulfonic acid (pTSA) was added to it and the mixture was stirred at 75° C.-80° C. for 40 h. 1H-NMR showed 85% conversion. More 2-chloro-3-hydroxypropionic acid (1.00 g, 8.00 mmol) was added to it and heated at 75° C.-80° C. for 20 h. 1H-NMR showed almost complete conversion. After cooling it down, the product was added with 100 mL of CH2Cl2. Organic phase was washed twice with 50 mL of dil. NaHCO3 aq. sol. and once with 50 mL of sat. NaCl aq. sol. and then dried over anhy. Na2SO4. After filtration and removing the solvent by rotary evaporation, yield=7.76 g (78%). It was used for the next reaction without further purification. 1H-NMR (CDCl3, 7.27 ppm): 2.18-2.40 (broad, —OH), 3.97 (m, —CH2OH), 4.21 (m, —CO2CH2), 4.39 (m, —CHCl).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08524942B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-dd70758721d642d29d1cf230ba39a7bb |
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| 출처 메모 | uspto-grants-2013_09 |
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