Potassium Carbonate → (3R,3aS,6aR)-hexahydrofuro(2,3-b)furan-3-ol

HRID 1505578

반응식

HRID 1505578 반응식
C([O:4][C@@H:5]1[C@H:12]2[C@H:8]([O:9][CH2:10][CH2:11]2)[O:7][CH2:6]1)(=O)C.C(=O)([O-])[O-].[K+].[K+]>CO.ClCCl>[O:7]1[C@H:8]2[O:9][CH2:10][CH2:11][C@H:12]2[C@@H:5]([OH:4])[CH2:6]1

참가 물질

5

반응물 2

HCID 11430Potassium CarbonateHCID 59959307(3R,3aS,6aR)-Hexahydrofuro[2,3-b]furan-3-yl acetate

생성물 1

HCID 9942150(3R,3aS,6aR)-hexahydrofuro(2,3-b)furan-3-ol수율 99.2%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

반응 조건

온도
30 °C

실험 절차

(3R,3aS,6aR)-Hexahydrofuro[2,3-b]furan-3-yl acetate (II, 14.0 g) was dissolved in methanol (42 mL). Potassium carbonate (0.34 g) was added and stirred at 25-35° C. for 6-8 hours. Methanol Was distilled out completely under vacuum, to the distillate methylenedichloride (28 mL) was added, stirred the mass for 30 minutes and again distilled the solvent to get residue. Dissolved the residue in dichloromethane (56 mL), the resultant solution was treated with carbon and the solvent was completely distilled out get title compound I (yield 10.5 g).

후처리

  1. distillationMethanol Was distilled out completely under vacuum, to the distillate methylenedichloride (28 mL)
  2. additionwas added
  3. stirringstirred the mass for 30 minutes
  4. distillationagain distilled the solvent
  5. customto get residue
  6. distillationthe solvent was completely distilled out

출처 및 근거

ORD 기록
ord-55ddae41e48d4439bdad97b451074da2
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09216990B2

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