Potassium Carbonate → HCID 58079363、化合物

HRID 1027368ノート

反応式

HRID 1027368 の反応式
C[O:2][C:3]1[CH2:8][C:7]([O:9]C)=[CH:6][CH:5]([CH2:11][CH:12]2[O:16][CH2:15][CH2:14][O:13]2)[CH:4]=1.C(=O)([O-])[O-].[K+].[K+]>Cl.O1CCCC1>[O:13]1[CH2:14][CH2:15][O:16][CH:12]1[CH2:11][CH:5]1[CH2:6][C:7](=[O:9])[CH2:8][C:3](=[O:2])[CH2:4]1

参加物

5

実験手順

A solution of 2-(3,5-dimethoxycyclohexa-2,5-dienylmethyl)-[1,3]-dioxolane (730 mgs, 3.2 mmol) in a mixture of 10% aqueous hydrochloric acid (2.9 ml) and tetrahydrofuran (29 ml) is stirred at room temperature for ¾ hour. The reaction mixture is poured into an aqueous solution of saturated potassium carbonate and extracted with ethyl acetate. The organic extract is discarded. The aqueous extract is acidified with dilute aqueous hydrochloric acid and extracted with ethyl acetate. The organic extract is dried over anhydrous magnesium sulfate, filtered and then filtrate evaporated in vacuo to give 5-([1,3]-dioxolan-2-ylmethyl)-cyclohexane-1,3-dione as a white solid, used without further purification in the next step.

後処理

  1. extractionextracted with ethyl acetate
  2. extractionThe organic extract
  3. extractionThe aqueous extract
  4. extractionextracted with ethyl acetate
  5. extractionThe organic extract
  6. dry with materialis dried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. customfiltrate evaporated in vacuo

出典と根拠

ORDレコード
ord-9a346089337244ef946783237a28a2a8
出典データセット
uspto-grants-2014_05
特許番号
US08735322B2

反応ノート

読み込み中…