Hydrochloric Acid → 2,2'-methanediyldicyclohexanone

HRID 1105964ノート

反応式

HRID 1105964 の反応式
CC1[O:7][CH:6]([CH3:8])OC(C)O1.[OH-].[K+].[C:12]1(=[O:18])[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1.Cl>CO>[CH2:14]([CH:13]1[CH2:12][CH2:17][CH2:16][CH2:8][C:6]1=[O:7])[CH:13]1[CH2:14][CH2:15][CH2:16][CH2:17][C:12]1=[O:18]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 7967CyclohexanoneHCID 14797Potassium HydroxideHCID 31264Paraldehyde

生成物 1

HCID 37551872,2'-methanediyldicyclohexanone収率 64%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

A mixture comprising 68 g of paraldehyde, 6 g of caustic potash and 188 g of methanol was added dropwise to a solution comprising 1,000 g of cyclohexanone and 188 g of methanol at 60°-70° C. over a period of 2 hours, and the resulting mixture was stirred for another 3 hours at 60°-70° C. Thereafter, the reaction mixture was decomposed with dilute hydrochloric acid, extracted with ether, washed first with 3% aqueous sodium carbonate, then with saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate. After recovering the solvent, the dried product was distilled under vacuum to provide 340 g (yield: 64%) of a fraction boiling at 135°-145° C./3 mm Hg.

後処理

  1. additionwas added dropwise to a solution
  2. customat 60°-70° C.
  3. customof 2 hours
  4. extractionextracted with ether
  5. washwashed first with 3% aqueous sodium carbonate
  6. dry with materialwith saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate
  7. customAfter recovering the solvent
  8. distillationthe dried product was distilled under vacuum
  9. customto provide 340 g (yield: 64%) of a fraction boiling at 135°-145° C./3 mm Hg

出典と根拠

ORDレコード
ord-73748befc89a462d918191ee1065e858
出典データセット
uspto-grants-1982_01
特許番号
US04310685

反応ノート

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