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

HRID 37188ノート

反応式

HRID 37188 の反応式
[CH3:1][O:2][C:3]1[CH:36]=[CH:35][CH:34]=[CH:33][C:4]=1[O:5][CH2:6][CH2:7][N:8]([CH3:32])[CH2:9][CH2:10][CH2:11][NH:12]C(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.CO.Cl>O>[CH3:1][O:2][C:3]1[CH:36]=[CH:35][CH:34]=[CH:33][C:4]=1[O:5][CH2:6][CH2:7][N:8]([CH3:32])[CH2:9][CH2:10][CH2:11][NH2:12]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 19934803HCID 19934803、化合物

生成物 1

HCID 19934807N-[2-(2-Methoxyphenoxy)ethyl]-N-methyl-1,3-propanediamine収率 87.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

12.9 g (0.0268 mol) of N-[2-(2-methoxyphenoxy)ethyl]-N-methyl-N'-(triphenylmethyl)-1,3-propanediamine and 250 ml of methanol are introduced into a 1 l round-bottomed flask. A stream of gaseous hydrochloric acid is passed for 15 min while cooling with a mixture of water and ice. The mixture is allowed to return to room temperature and is then brought to the reflux temperature for 7.5 h. The mixture is concentrated to dryness and the residue is taken up in ethanol and concentrated again. The residue is taken up in water, the mixture is basified, the supernatant oil is taken up in dilute hydrochloric acid and extraction is carried out with diethyl ether. The acidic aqueous phase is then treated with sodium hydroxide until the pH is basic and extraction is carried out with dichloromethane. The organic phase is washed with water, dried over sodium sulphate and concentrated under reduced pressure. There are obtained 5.6 g of a yellow oil which is used as is in the following stage.

後処理

  1. customto return to room temperature
  2. concentrationThe mixture is concentrated to dryness
  3. concentrationconcentrated again
  4. extractionextraction
  5. additionThe acidic aqueous phase is then treated with sodium hydroxide until the pH
  6. extractionextraction
  7. washThe organic phase is washed with water
  8. dry with materialdried over sodium sulphate
  9. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-077245972e6e4acc9eccd5ef240f35a5
出典データセット
uspto-grants-1995_05
特許番号
US05420130

反応ノート

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