Hydrochloric Acid → 4-Benzyl-4-dimethylaminomethyl-1-methylamino-cyclohexane carbonitrile

HRID 76932ノート

反応式

HRID 76932 の反応式
[CH3:1][NH2:2].[CH2:3]([C:10]1([CH2:17][N:18]([CH3:20])[CH3:19])[CH2:15][CH2:14][C:13](=O)[CH2:12][CH2:11]1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.Cl.[C-:22]#[N:23].[K+]>CO.O>[CH2:3]([C:10]1([CH2:17][N:18]([CH3:20])[CH3:19])[CH2:15][CH2:14][C:13]([NH:23][CH3:22])([C:1]#[N:2])[CH2:12][CH2:11]1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 6329MethylamineHCID 9032Potassium CyanideHCID 686332214-Benzyl-4-((dimethylamino)methyl)cyclohexanone

生成物 1

HCID 686305894-Benzyl-4-dimethylaminomethyl-1-methylamino-cyclohexane carbonitrile

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

40% aqueous methylamine solution (15.3 mL, 121 mmol) and 4-benzyl-4-((dimethylamino)methyl)cyclohexanone (6.20 g, 25.3 mmol) dissolved in methanol (25 mL) were added to a solution of 4N hydrochloric acid (6.6 mL) and methanol (4.00 mL) cooled to 0° C. The reaction mixture was then mixed with potassium cyanide (4.00 g, 60 mmol) and stirred for 5 d at room temperature. For work up the mixture was diluted with water (180 mL) and extracted with ether (3×100 mL). The combined organic phases were dried over Na2SO4, filtered and concentrated until dry in a vacuum.

後処理

  1. extractionextracted with ether (3×100 mL)
  2. dry with materialThe combined organic phases were dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customuntil dry in a vacuum

出典と根拠

ORDレコード
ord-2ce5109d290e4d4483de4989ceeee14b
出典データセット
uspto-grants-2014_09
特許番号
US08835689B2

反応ノート

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