Sodium Hydroxide → 3'-Chloro-4'-(4-methyl-1-piperazinyl)acetophenone

HRID 972679

反応式

HRID 972679 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:9](=[O:11])[CH3:10])[CH:5]=[CH:6][C:7]=1Cl.[CH3:12][N:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1.[OH-].[Na+]>O>[Cl:1][C:2]1[CH:3]=[C:4]([C:9](=[O:11])[CH3:10])[CH:5]=[CH:6][C:7]=1[N:16]1[CH2:17][CH2:18][N:13]([CH3:12])[CH2:14][CH2:15]1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 531671-MethylpiperazineHCID 75841Ethanone, 1-(3,4-dichlorophenyl)-

生成物 1

HCID 214045803'-Chloro-4'-(4-methyl-1-piperazinyl)acetophenone

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

3',4'-Dichloroacetophenone (9.65 g., 0.05 mole) and N-methylpiperazine (10 g., 0.1 mole) are refluxed (165° C.) for 24 hours. The solution is cooled and 100 ml. water containing 2 g. of sodium hydroxide is added. The oil is decanted and diluted with 200 ml. of toluene and washed first with dilute alkali then several times with water. The toluene layer is dried with magnesium sulfate and evaporated in vacuo to an oil. The residue is distilled 146°-150° at 0.1-0.3 mm., yield 3.0 g. This product is dissolved in ethyl ether and converted to the hydrochloride using isopropanolic hydrogen chloride and the salt crystallized from acetonitrile. The purified salt is reconverted to the base with dilute sodium hydroxide. The product is extracted using ethyl ether, separated, dried, evaporated to dryness to give 3'-chloro-4'-(4-methyl-1-piperazinyl)acetophenone as a yellow oil.

後処理

  1. temperatureThe solution is cooled
  2. customThe oil is decanted
  3. additiondiluted with 200 ml
  4. washof toluene and washed first with dilute alkali
  5. dry with materialThe toluene layer is dried with magnesium sulfate
  6. customevaporated in vacuo to an oil
  7. distillationThe residue is distilled 146°-150° at 0.1-0.3 mm
  8. dissolutionThis product is dissolved in ethyl ether
  9. customthe salt crystallized from acetonitrile
  10. extractionThe product is extracted
  11. customseparated
  12. customdried
  13. customevaporated to dryness

出典と根拠

ORDレコード
ord-0b4d76a994e04d15b9d3ca5c9f0601d9
出典データセット
uspto-grants-1977_10
特許番号
US04053470

関連ノート

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