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 | Monosodium phosphate | HCID 23672064 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | (3R,3aS,6aR)-Hexahydrofuro[2,3-b]furan-3-yl acetate | HCID 59959307 | 34.8% |
반응 단계
To the buffer solution (104.3 g of sodium dihydrogen orthophosphate dissolved in 530 mL of water & pH adjusted to 6.0-6.5 with saturated sodium bicarbonate solution (68 g in 680 mL water) solution) hexahydrofuro[2,3-b]furan-3-yl acetate (III, 115 g) and CAL-B (17.25 g) was added at 25-35° C., heated to 38-45° C. and stirred for 24 hours. CAL-B (17.25 g) was added stirred for 16 hours, again CAL-B (11.5 g) was added at 38-45° C. and stirred for 16 hours (pH should maintain 6.0-6.5). The reaction mass was cooled to 20-30° C., methylenedichloride (1150 mL) was added to the mass and stirred for 30 minutes. The reaction mass was filtered through hyflowbed then separated the organic layer and washed with 10% sodium chloride solution (575 mL). Organic layer was distilled completely under vacuum to get title compound II (yield 40.0 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09216990B2 |
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| 출처 데이터셋 | uspto-grants-2015_12 |
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| ORD ID | ord-339df309fb8d419782686a04b83487bf |
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| 출처 메모 | uspto-grants-2015_12 |
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