関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Hexahydrofuro[2,3-b]furan-3-yl acetate | HCID 21869022 | — |
| 反応物 | Sodium Phosphate, Monobasic, Dihydrate | HCID 23673460 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (3R,3aS,6aR)-Hexahydrofuro[2,3-b]furan-3-yl acetate | HCID 59959307 | 42.7% |
反応手順
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%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08841467B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-6834833e4545493db374aef79cde797e |
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| 出典メモ | uspto-grants-2014_09 |
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