참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | Hexahydrofuro[2,3-b]furan-3-yl acetate | HCID 21869022 | — |
| 반응물 | Sodium Phosphate, Monobasic, Dihydrate | HCID 23673460 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | (3R,3aS,6aR)-Hexahydrofuro[2,3-b]furan-3-yl acetate | HCID 59959307 | 42.7% |
반응 단계
Hexahydrofuro[2,3-b]furan-3-yl acetate (124 g) to the RB flask along with buffer solution (118 g Sodium dihydrogen phosphate dihydrate dissolved in 600 ml water & pH adjusted to 6.5 with saturated NaHCO3 aqueous solution). CAL-B enzyme (19.5 g) was added to the reaction mass and stirred at 40-45° C. Reaction was monitored by Chiral-GC. Reaction was cooled to room temp., dichloromethane (1300 ml) was charged to reaction mass and filtered through hyflow bed. Dichloromethane layer was separated and washed with Sodium chloride solution (10%, 650 ml) and water (3×650 ml). Dichloromethane layer was concentrated under vacuum to get residue of (3R,3aS,6aR)-Hexahydrofuro[2,3-b]furan-3-yl acetate (Yield 53 g). Further, the product was purified by fractional distillation under vacuum at 98-118° C. to get main fraction 39.5 g having purity 97.98%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08841467B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-6834833e4545493db374aef79cde797e |
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| 출처 메모 | uspto-grants-2014_09 |
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