1,4-Dioxane hydrochloride → n,n-Dipropylpropane-1,3-diamine

HRID 1173855ノート

反応式

HRID 1173855 の反応式
[CH2:1]([N:4]([CH2:16][CH2:17][CH3:18])[CH2:5][CH2:6][CH2:7][NH:8]C(OC(C)(C)C)=O)[CH2:2][CH3:3].Cl.O1CCOCC1>CO>[CH2:16]([N:4]([CH2:1][CH2:2][CH3:3])[CH2:5][CH2:6][CH2:7][NH2:8])[CH2:17][CH3:18]

参加物

4

反応物 2

HCID 204431481,4-Dioxane hydrochlorideHCID 23079224N,N-dipropyl-N'-Boc-1,3-propanediamine

生成物 1

HCID 239005n,n-Dipropylpropane-1,3-diamine収率 44.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

The compound (2.67 g) obtained in Example 22-2 was dissolved in anhydrous methanol (2.0 ml) and then added with a 4 mol/l hydrogen chloride/dioxane solution (20.0 ml), followed by stirring at room temperature for 1.5 hours. After completion of the reaction, the solvent was distilled off. Then, the residue was added with a 1 mol/l sodium hydroxide aqueous solution and extracted with dichloromethane. The extract was washed with distilled water and saturated saline solution, and then the organic layer was dried with anhydrous sodium sulfate. Subsequently, the solvent was distilled off, thereby obtaining the subject compound (726 mg) as a pale-yellow liquid.

後処理

  1. customAfter completion of the reaction
  2. distillationthe solvent was distilled off
  3. additionThen, the residue was added with a 1 mol/l sodium hydroxide aqueous solution
  4. extractionextracted with dichloromethane
  5. washThe extract was washed with distilled water and saturated saline solution
  6. dry with materialthe organic layer was dried with anhydrous sodium sulfate
  7. distillationSubsequently, the solvent was distilled off

出典と根拠

ORDレコード
ord-9effc3af86fb4dc4b0b5ace4280fee08
出典データセット
uspto-grants-2010_11
特許番号
US07833991B2

反応ノート

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