Acetone → 4-Methylamino-4-phenylcyclohexanone hydrochloride

HRID 1462511ノート

反応式

HRID 1462511 の反応式
[CH3:1][NH:2][C:3]1([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:8][CH2:7][C:6](=[O:9])[CH2:5][CH2:4]1.[ClH:16].CC(C)=O.C(=O)(O)[O-].[Na+]>C(OCC)C.C(Cl)Cl>[ClH:16].[CH3:1][NH:2][C:3]1([C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)[CH2:8][CH2:7][C:6](=[O:9])[CH2:5][CH2:4]1

参加物

7

反応物 4

HCID 180AcetoneHCID 313Hydrochloric Acid2 回HCID 516892Sodium BicarbonateHCID 133452704-Methylamino-4-phenylcyclohexanone

生成物 1

HCID 204533474-Methylamino-4-phenylcyclohexanone hydrochloride収率 74%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒3 回HCID 6344Dichloromethane溶媒

実験手順

A reaction mixture consisting of 1.0 gm. (0.0035 mole) of 4-methylamino-4-phenylcyclohexanone, ethylene ketal, hydrochloride (prepared in Example 17, Part G, above) 2.0 ml. of 2.5 N hydrochloric acid, and 20 ml. acetone is stirred continuously for eighteen (18) hours, at 25° C. The reaction mixture is then made basic by adding solid sodium bicarbonate, and most of the solvent is removed by evaporation under reduced pressure. The concentrated material thus obtained is ectracted four times with 20 ml. portions of methylene chloride. the extracts are combined and the methylene chloride is removed by evaporation under reduced pressure. A gummy residue is obtained that is dissolved in diethyl ether. The ether solution is treated with hydrogen chloride in ether. A precipitate forms which is collected on a filter and recrystallized from a mixture of methylene chloride and ethyl acetate. There is thus obtained 0.53 gm. (74% yield) of 4-methylamino-4-phenylcyclohexanone hydrochloride having a melting range from 218° to 220° C.

後処理

  1. custommost of the solvent is removed by evaporation under reduced pressure
  2. customThe concentrated material thus obtained
  3. customthe methylene chloride is removed by evaporation under reduced pressure
  4. customA gummy residue is obtained
  5. customA precipitate forms which is collected on
  6. filtrationa filter
  7. customrecrystallized from a mixture of methylene chloride and ethyl acetate

出典と根拠

ORDレコード
ord-bb5a293ac1934ad1beabbc33dbf5f5b2
出典データセット
uspto-grants-1984_07
特許番号
US04460604

反応ノート

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