Dichloromethane → 2-Methylene-3-quinuclidone

HRID 745539

反応式

HRID 745539 の反応式
Cl.O.O.[CH2:4]=[C:5]1[C:10](=[O:11])[CH:9]2[CH2:12][CH2:13][N:6]1[CH2:7][CH2:8]2.C(=O)([O-])[O-].[K+].[K+].C(Cl)Cl>O>[CH2:4]=[C:5]1[C:10](=[O:11])[CH:9]2[CH2:12][CH2:13][N:6]1[CH2:7][CH2:8]2

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 219542752-Methylene-3-quinuclidinone dihydrate hydrochloride

生成物 1

HCID 3229732-Methylene-3-quinuclidone

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Suspend 95.4 g (0.455 mole) 2-methylene-3-quinuclidinone dihydrate hydrochloride in a solution of 255 g (1.85 moles) anhydrous potassium carbonate dissolved in 350 ml H2O. When the suspension clears add 500 ml methylene chloride and mix the 2-phase system overnight using a mechanical stirrer. Separate the layers and dry the methylene chloride layer over potassium carbonate. Remove the solvents in vacuo to obtain the title compound. Repeat the extraction until most of the product is collected.

後処理

  1. additionmix the 2-phase system overnight
  2. customSeparate the layers
  3. dry with materialdry the methylene chloride layer over potassium carbonate
  4. customRemove the solvents in vacuo

出典と根拠

ORDレコード
ord-8487bf1433834c318e8cfa3a4af4c32e
出典データセット
uspto-grants-1986_07
特許番号
US04599344

関連ノート

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