참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethanolamine | HCID 700 | — |
| 반응물 | 2,3,3,3-Tetrafluoro-2-(1,1,2,2,3,3,3-heptafluoropropoxy)propanoyl fluoride | HCID 102740 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | N-(perfluoro-2-methyl-3-oxahexanoyl)-2-aminoethanol | HCID 86641009 | 335% |
반응 단계
A mixture of ethanolamine (13 g, 28 mmol) and ether (30 mL) was cooled to 15° C. Perfluoro-2-methyl-3-oxahexanoyl fluoride (33 g in ether 50 mL) was added dropwise to keep the reaction temperature below 25° C. After the addition, the reaction mixture was stirred at room temperature for one hour. The solid was removed by filtration and the filtrate was washed with hydrochloric acid (0.5N, 30 mL), water (2 times 30 mL), sodium hydrogen carbonate solution (0.5N, 20 mL), water (30 mL), and sodium chloride solution (saturated, 20 mL). It was then concentrated and dried in vacuum over night at room temperature to give N-(perfluoro-2-methyl-3-oxahexanoyl)-2-aminoethanol as a white solid 35 g, yield 95%. mp. 69-72° C. 1H NMR (CDCl3) δ 1.67 (bs, 1H), 3.57 (m, 2H), 3.80 (t, J=5 Hz, 2H), 6.91 (bs, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08022107B2 |
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| 출처 데이터셋 | uspto-grants-2011_09 |
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| ORD ID | ord-e1ed8edad1f443aba17cff92e0b96795 |
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| 출처 메모 | uspto-grants-2011_09 |
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