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

HRID 1505578

反応式

HRID 1505578 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
30 °C

実験手順

(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).

後処理

  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

出典と根拠

ORDレコード
ord-55ddae41e48d4439bdad97b451074da2
出典データセット
uspto-grants-2015_12
特許番号
US09216990B2

関連ノート

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