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

HRID 78757

反応式

HRID 78757 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>[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

4

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 1

HCID 887Methanol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 (14.0 g) was dissolved in Methanol (42 ml). Potassium carbonate (0.34 g) was added to the reaction mass. Reaction mass was stirred at 25-35° C. till the completion of reaction. Reaction mass was concentrated to residue under vacuum at 40-45° C. Dichloromethane (42 ml) was charged to residue along with activated carbon (0.7 g) and stirred for 1 hr and then filtered through hyflow bed. Filtrate was concentrated to residue to get (3R,3aS,6aR)-Hexahydrofuro[2,3-b]furan-3-ol (Yield 10.5 g)

後処理

  1. customReaction mass
  2. customReaction mass
  3. concentrationwas concentrated to residue under vacuum at 40-45° C
  4. additionDichloromethane (42 ml) was charged to residue along with activated carbon (0.7 g)
  5. stirringstirred for 1 hr
  6. filtrationfiltered through hyflow bed
  7. concentrationFiltrate was concentrated to residue

出典と根拠

ORDレコード
ord-594b79cde7d44dfc8ccef9e7d58fa58a
出典データセット
uspto-grants-2014_09
特許番号
US08841467B2

関連ノート

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