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1,4-Dioxane hydrochloride → [(4-Aminomethyl-benzyl)-(4-dipropylamino-butyl)-amino]-acetic acid ethyl ester

HRID 2080858
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HRID 2080858 반응식
[CH2:1]([O:3][C:4](=[O:34])[CH2:5][N:6]([CH2:18][C:19]1[CH:24]=[CH:23][C:22]([CH2:25][NH:26]C(OC(C)(C)C)=O)=[CH:21][CH:20]=1)[CH2:7][CH2:8][CH2:9][CH2:10][N:11]([CH2:15][CH2:16][CH3:17])[CH2:12][CH2:13][CH3:14])[CH3:2].Cl.O1CCOCC1>C(O)C>[CH2:1]([O:3][C:4](=[O:34])[CH2:5][N:6]([CH2:18][C:19]1[CH:20]=[CH:21][C:22]([CH2:25][NH2:26])=[CH:23][CH:24]=1)[CH2:7][CH2:8][CH2:9][CH2:10][N:11]([CH2:12][CH2:13][CH3:14])[CH2:15][CH2:16][CH3:17])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 204431481,4-Dioxane hydrochlorideHCID 67103729[[4-(t-Butoxycarbonylamino-methyl)-benzyl]-(4-dipropylamino-butyl)-amino]-acetic acid ethyl ester

생성물 1

HCID 59850563[(4-Aminomethyl-benzyl)-(4-dipropylamino-butyl)-amino]-acetic acid ethyl ester수율 97.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

The compound (21.265 g) obtained in Example 72-1 was dissolved in ethanol (100 ml) and added with a 4 mol/l hydrogen chloride/dioxane solution (140 ml) and the whole was stirred at room temperature for 1 hour. Subsequently, the solution was stirred at 40° C. for 1 hour. After completion of the reaction, the solvent was distilled off. The resultant was added with a 1 mol/l sodium hydroxide aqueous solution to make the pH thereof to 12. The solution was subjected to extraction with chloroform and dried with magnesium sulfate. The solvent was distilled off, thereby obtaining the subject compound (16.46 g) as a colorless oily substance.

후처리

  1. stirringSubsequently, the solution was stirred at 40° C. for 1 hour
  2. customAfter completion of the reaction
  3. distillationthe solvent was distilled off
  4. additionThe resultant was added with a 1 mol/l sodium hydroxide aqueous solution
  5. extractionThe solution was subjected to extraction with chloroform
  6. dry with materialdried with magnesium sulfate
  7. distillationThe solvent was distilled off

출처 및 근거

ORD 기록
ord-47c3fc6e4ed844338ed95155a7573b82
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07932281B2

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