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

HRID 407839

반응식

HRID 407839 반응식
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

참가 물질

4

반응물 3

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-28b27e2a961044e8990a77243e81ff8d
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08754242B2

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