Iodine → 5-Methoxy-10-oxa-tricyclo[5.2.1.0*2,6*]dec-4-en-3-one

HRID 407839

反応式

HRID 407839 の反応式
II.[CH:3]12[O:12][CH:9]([CH2:10][CH2:11]1)[CH:8]1[CH:4]2[C:5](=[O:14])[CH2:6][C:7]1=[O:13].[CH3:15]O>>[CH3:15][O:14][C:5]1[CH:4]2[CH:8]([CH:9]3[O:12][CH:3]2[CH2:11][CH2:10]3)[C:7](=[O:13])[CH:6]=1

参加物

4

反応物 3

HCID 807IodineHCID 887MethanolHCID 5935195110-Oxa-tricyclo[5.2.1.0*2,6*]decane-3,5-dione

生成物 1

HCID 672834435-Methoxy-10-oxa-tricyclo[5.2.1.0*2,6*]dec-4-en-3-one

実験手順

Iodine (0.10 g, 0.38 mmol) is added to a solution of (1RS,2SR,6RS,7SR)-10-oxa-tricyclo[5.2.1.02,6]decane-3,5-dione (2.1 g, 12.65 mmol) in methanol (50 ml) and the reaction mixture is stirred for 2 hours at room temperature. The solvent is then removed under reduced pressure, dichloromethane is added and the organic layer is washed with saturated aqueous sodium thiosulfate solution, water and brine. The organic layer is dried over anhydrous magnesium sulfate, filtered and the filtrate is evaporated under reduced pressure to give (1RS,2SR,6RS,7SR)-5-methoxy-10-oxatricyclo[5.2.1.02,6]dec-4-en-3-one and used without further purification in the next step.

後処理

  1. customThe solvent is then removed under reduced pressure, dichloromethane
  2. additionis added
  3. washthe organic layer is washed with saturated aqueous sodium thiosulfate solution, water and brine
  4. dry with materialThe organic layer is dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customthe filtrate is evaporated under reduced pressure

出典と根拠

ORDレコード
ord-28b27e2a961044e8990a77243e81ff8d
出典データセット
uspto-grants-2014_06
特許番号
US08754242B2

関連ノート

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