1,4-Dioxane hydrochloride → n,n-Dipropylpropane-1,3-diamine
반응식
[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]참가 물질
4
실험 절차
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.
후처리
- customAfter completion of the reaction
- distillationthe solvent was distilled off
- additionThen, the residue was added with a 1 mol/l sodium hydroxide aqueous solution
- extractionextracted with dichloromethane
- washThe extract was washed with distilled water and saturated saline solution
- dry with materialthe organic layer was dried with anhydrous sodium sulfate
- distillationSubsequently, the solvent was distilled off
출처 및 근거
- ORD 기록
- ord-9effc3af86fb4dc4b0b5ace4280fee08
- 출처 데이터셋
- uspto-grants-2010_11
- 특허 번호
- US07833991B2
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