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Hydrochloric Acid → N-Methyl-N-[2-(3,4-dimethoxyphenyl)ethyl]-2-methyl-1,3-propanediamine

HRID 974996
ノート
印刷プレビュー

反応式

HRID 974996 の反応式
[CH3:1][N:2]([CH2:15][CH:16]([CH3:19])[C:17]#[N:18])[CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([O:11][CH3:12])=[C:7]([O:13][CH3:14])[CH:6]=1.Cl>C(O)C.[Pt]=O>[CH3:1][N:2]([CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([O:11][CH3:12])=[C:7]([O:13][CH3:14])[CH:6]=1)[CH2:15][CH:16]([CH3:19])[CH2:17][NH2:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 199703153-[N-methyl-N-(2-(3,4-dimethoxyphenyl)ethyl)amino]-2-methylpropionitrile

生成物 1

HCID 15045284N-Methyl-N-[2-(3,4-dimethoxyphenyl)ethyl]-2-methyl-1,3-propanediamine収率 92.9%

試薬・触媒・溶媒 2

HCID 82844Platinum oxide (PtO)触媒HCID 702Ethanol溶媒

実験手順

2.1 g of the above nitrile and 0.2 ml of concentrated hydrochloric acid were dissolved in 30 ml of ethanol, followed by the addition of 0.2 g of platinum oxide to carry out hydrogenation under a hydrogen pressure of 2.1 kg/cm2. The reaction mixture was filtered to remove the catalyst. The filtrate was distilled under a reduced pressure to remove the ethanol. The residue was made alkaline with a dilute solution of caustic soda. The aqueous layer was extracted with dichloromethane. The extract was washed with water, dried over magnesium sulfate and distilled under a reduced pressure to obtain 1.98 g of the title compound as a pale yellow oil (yield: 38%).

後処理

  1. filtrationThe reaction mixture was filtered
  2. customto remove the catalyst
  3. distillationThe filtrate was distilled under a reduced pressure
  4. customto remove the ethanol
  5. extractionThe aqueous layer was extracted with dichloromethane
  6. washThe extract was washed with water
  7. dry with materialdried over magnesium sulfate
  8. distillationdistilled under a reduced pressure

出典と根拠

ORDレコード
ord-b9ec535add8c4572b16755b419caa99a
出典データセット
uspto-grants-1997_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05607953

反応ノート

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