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

HRID 2080858
ノート
印刷プレビュー

反応式

HRID 2080858 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-47c3fc6e4ed844338ed95155a7573b82
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07932281B2

反応ノート

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