Methanol → 3-[(2-Pyridin-3-ylethyl)pyridin-4-ylmethylamino]propan-1-ol

HRID 68996ノート

反応式

HRID 68996 の反応式
CO.Cl.CO.[N:6]1[CH:11]=[CH:10][CH:9]=[C:8]([CH2:12][CH2:13][N:14]([CH2:25][C:26]2[CH:31]=[CH:30][N:29]=[CH:28][CH:27]=2)[CH2:15][CH2:16][CH2:17][O:18]C2CCCCO2)[CH:7]=1>C(N(CC)CC)C>[N:6]1[CH:11]=[CH:10][CH:9]=[C:8]([CH2:12][CH2:13][N:14]([CH2:25][C:26]2[CH:31]=[CH:30][N:29]=[CH:28][CH:27]=2)[CH2:15][CH2:16][CH2:17][OH:18])[CH:7]=1

参加物

5

反応物 3

HCID 887MethanolHCID 21893726Hydrochloride methanol2 回HCID 66960900(2-Pyridin-3-ylethyl)pyridin-4-ylmethyl-[3-(tetrahydropyran-2-yloxy)propyl]amine

生成物 1

HCID 669609373-[(2-Pyridin-3-ylethyl)pyridin-4-ylmethylamino]propan-1-ol収率 103.4%

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

A 2N-hydrogen chloride methanol solution (1.2 ml) was added to a methanol solution (4 ml) of (2-pyridin-3-ylethyl)pyridin-4-ylmethyl-[3-(tetrahydropyran-2-yloxy)propyl]amine (236 mg). The mixture was stirred at room temperature overnight. A 2N-hydrogen chloride methanol solution (0.5 ml) was added thereto, and the mixture was further stirred at 50° C. for 3 hours. Triethylamine (0.64 ml) was added to the reaction mixture, and the mixture was condensed under reduced pressure. The residue was purified by basic silica gel column chromatography (dichloromethane). The purified product was condensed under reduced pressure to give the title compound (186.3 mg) as an orange oily matter.

後処理

  1. stirringthe mixture was further stirred at 50° C. for 3 hours
  2. customcondensed under reduced pressure
  3. customThe residue was purified by basic silica gel column chromatography (dichloromethane)
  4. customcondensed under reduced pressure

出典と根拠

ORDレコード
ord-b69f6ab5a3be41fca59b82a379afdf31
出典データセット
uspto-grants-2014_09
特許番号
US08822453B2

反応ノート

読み込み中…