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Dimethyl-(2-pyridin-3-yl-cyclohex-2-enylmethyl)amine hydrochloride → cis-Dimethyl-(2-pyridin-3-yl-cyclohexylmethyl)amine hydrochloride

HRID 131530
ノート
印刷プレビュー

反応式

HRID 131530 の反応式
[ClH:1].[CH3:2][N:3]([CH3:17])[CH2:4][CH:5]1[CH2:10][CH2:9][CH2:8][CH:7]=[C:6]1[C:11]1[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=1>CO.[Pd]>[ClH:1].[CH3:2][N:3]([CH3:17])[CH2:4][C@@H:5]1[CH2:10][CH2:9][CH2:8][CH2:7][C@@H:6]1[C:11]1[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 69220584Dimethyl-(2-pyridin-3-yl-cyclohex-2-enylmethyl)amine hydrochloride

生成物 1

HCID 69223110cis-Dimethyl-(2-pyridin-3-yl-cyclohexylmethyl)amine hydrochloride収率 34.8%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

6.90 g dimethyl-(2-pyridin-3-yl-cyclohex-2-enylmethyl)amine hydrochloride were dissolved in 70 ml methanol and hydrogenated in the presence of 1.04 g palladium-on-active charcoal (10 percent by weight) for five hours under a hydrogen pressure of 2 bar. The mixture was then filtered, the filtrate was concentrated in vacuo, the residue was converted into the base with two molar sodium hydroxide solution and a mixture of equal volumes of ethyl acetate and tetrahydrofuran and the base was extracted with ethyl acetate. After drying and concentration, the residue (4.47 g) was chromatographed on silica gel with a mixture of equal volumes of methanol, ethyl acetate and n-hexane. The main fraction (3.72 g) was dissolved in approx. 40 ml acetone/ethanol (V/V=9:1), and half a molar equivalent of water and one molar equivalent of chlorotrimethylsilane were added. After the mixture had been stirred overnight, it was concentrated to dryness, the residue was treated in an ultrasonic bath with 72 ml THF and 18 ml ethanol for 30 minutes, the suspension was stirred overnight and filtered with suction and the residue was dried. 2.42 g cis-dimethyl-(2-pyridin-3-yl-cyclohexylmethyl)amine hydrochloride with a melting point of 219-222° C. were obtained.

後処理

  1. filtrationThe mixture was then filtered
  2. concentrationthe filtrate was concentrated in vacuo
  3. additiona mixture of equal volumes of ethyl acetate and tetrahydrofuran
  4. extractionthe base was extracted with ethyl acetate
  5. customAfter drying
  6. concentrationconcentration
  7. customthe residue (4.47 g) was chromatographed on silica gel with a mixture of equal volumes of methanol, ethyl acetate and n-hexane
  8. dissolutionThe main fraction (3.72 g) was dissolved in approx. 40 ml acetone/ethanol (V/V=9:1)
  9. additionhalf a molar equivalent of water and one molar equivalent of chlorotrimethylsilane were added
  10. concentrationit was concentrated to dryness
  11. additionthe residue was treated in an ultrasonic bath with 72 ml THF and 18 ml ethanol for 30 minutes
  12. stirringthe suspension was stirred overnight
  13. filtrationfiltered with suction
  14. customthe residue was dried

出典と根拠

ORDレコード
ord-b23fabec6d8f42a88149b368ffe5ffeb
出典データセット
uspto-grants-2008_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07384961B2

反応ノート

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