참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Ethyl chloroformate | HCID 10928 | — |
| 반응물 | Sodium borohydride | HCID 4311764 | — |
| 반응물 | 4-Ethoxycarbonylfuran-2-carboxylic acid | HCID 53429231 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 5-Hydroxymethyl-3-furancarboxylic acid ethyl ester | HCID 59478736 | 79% |
반응 단계
4-Ethoxycarbonylfuran-2-carboxylic acid (0.47 g, 2.53 mmol) was dissolved in tetrahydrofuran (10 mL), triethylamine (0.53 mL, 3.80 mmol) and ethyl chloroformate (0.29 mL, 3.04 mmol) were added at 0° C., and the mixture was stirred at room temperature for 1 hour. The reaction mixture was filtered through celite, water (0.23 mL, 12.7 mmol) and sodium borohydride (0.19 g, 5.06 mmol) were added to the filtrate, and the mixture was stirred overnight. 1N Hydrochloric acid was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate=50/50) to give the title compound (0.34 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09115107B2 |
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| 출처 데이터셋 | uspto-grants-2015_08 |
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| ORD ID | ord-3a93c60a729b416a9e05c29b80863f86 |
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| 출처 메모 | uspto-grants-2015_08 |
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