Toluene → 2-Methyl-1-[4-piperazinophenyl]-2-morpholino propan-1-one

HRID 1433108ノート

反応式

HRID 1433108 の反応式
[CH3:1][C:2]([N:13]1[CH2:18][CH2:17][O:16][CH2:15][CH2:14]1)([CH3:12])[C:3]([C:5]1[CH:10]=[CH:9][C:8](F)=[CH:7][CH:6]=1)=[O:4].[NH:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1.C1(C)C=CC=CC=1>ClCCl.[Cu]I>[CH3:1][C:2]([N:13]1[CH2:18][CH2:17][O:16][CH2:15][CH2:14]1)([CH3:12])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([N:19]2[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]2)=[CH:7][CH:6]=1)=[O:4]

参加物

6

反応物 3

HCID 1140TolueneHCID 4837PiperazineHCID 154053051-(4-Fluorphenyl)-2-methyl-2-morpholino-1-propanone

生成物 1

HCID 579346002-Methyl-1-[4-piperazinophenyl]-2-morpholino propan-1-one

試薬・触媒・溶媒 2

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)触媒HCID 6344Dichloromethane溶媒

実験手順

4.2 g of 2-methyl-1-[4-fluorophenyl]-2-morpholinopropan-1-one (0.0167 moles), 5.75 g of piperazine (0.0669 moles), 0.063 g of copper (I) iodide and 15 ml of toluene were mixed in a three necked flask equipped with a stirrer, nitrogen inlet, condenser, nitrogen outlet and a temperature probe. The mixture was heated to reflux for a total of 24 hours under a constant flow of nitrogen gas. The mixture was then cooled to room temperature, after which it was dissolved in 75 ml of dichloromethane. The mixture was then extracted with 100 ml of a saturated aqueous sodium chloride solution and then with 2×100 ml of water. The dichloromethane layer was then dried using anhydrous magnesium sulphate. The magnesium sulphate was removed by filtration and the organic solvent was then removed on a rotary evaporator to yield the product.

後処理

  1. customequipped with a stirrer, nitrogen inlet, condenser, nitrogen outlet
  2. temperatureThe mixture was heated
  3. temperatureto reflux for a total of 24 hours under a constant flow of nitrogen gas
  4. extractionThe mixture was then extracted with 100 ml of a saturated aqueous sodium chloride solution
  5. dry with materialThe dichloromethane layer was then dried
  6. customThe magnesium sulphate was removed by filtration
  7. customthe organic solvent was then removed on a rotary evaporator
  8. customto yield the product

出典と根拠

ORDレコード
ord-6b148dcc6da6414096c7c73de7ba7538
出典データセット
uspto-grants-2009_11
特許番号
US07612122B2

反応ノート

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