1,4-Dioxane hydrochloride → 1-{2-[(6-Aminohexanoyl)(methyl)amino]ethyl}piperidin-4-yl biphenyl-2-ylcarbamate dihydrochloride

HRID 446511ノート

反応式

HRID 446511 の反応式
[C:1]1([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH:7][C:8](=[O:35])[O:9][CH:10]1[CH2:15][CH2:14][N:13]([CH2:16][CH2:17][N:18]([C:20](=[O:34])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][NH:26]C(OC(C)(C)C)=O)[CH3:19])[CH2:12][CH2:11]1.[ClH:42].O1CCOCC1>O1CCOCC1>[ClH:42].[ClH:42].[C:1]1([C:36]2[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=2)[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH:7][C:8](=[O:35])[O:9][CH:10]1[CH2:11][CH2:12][N:13]([CH2:16][CH2:17][N:18]([C:20](=[O:34])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][NH2:26])[CH3:19])[CH2:14][CH2:15]1

参加物

4

反応物 2

HCID 204431481,4-Dioxane hydrochlorideHCID 666716851-{2-[{6-[(tert-Butoxycarbonyl)amino]hexanoyl}(methyl)amino]ethyl}piperidin-4-yl biphenyl-2-ylcarbamate

生成物 1

HCID 666717251-{2-[(6-Aminohexanoyl)(methyl)amino]ethyl}piperidin-4-yl biphenyl-2-ylcarbamate dihydrochloride収率 105.9%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

The compound (1.59 g, 2.80 mmol) obtained in Example 11b was dissolved in 1,4-dioxane (7 mL), 4 N hydrochloric acid-dioxane (7.00 mL, 28.0 mmol) was added under ice cooling, and the mixture was stirred at room temperature for 20 minutes. Since insoluble material was precipitated, methanol (4 mL) was added, and the mixture was stirred at room temperature for 40 minutes. The solvent was evaporated under reduced pressure to give the title compound (1.60 g; yield, 100%) as a white solid.

後処理

  1. customSince insoluble material was precipitated
  2. additionmethanol (4 mL) was added
  3. stirringthe mixture was stirred at room temperature for 40 minutes
  4. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-9cd9c3d50dab49938357f0c0383896cc
出典データセット
uspto-grants-2013_07
特許番号
US08476253B2

反応ノート

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