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

HRID 1183076노트

반응식

HRID 1183076 반응식
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

참가 물질

5

반응물 3

HCID 887MethanolHCID 21893726Hydrochloride methanol2회HCID 66960900(2-Pyridin-3-ylethyl)pyridin-4-ylmethyl-[3-(tetrahydropyran-2-yloxy)propyl]amine

생성물 1

HCID 669609373-[(2-Pyridin-3-ylethyl)pyridin-4-ylmethylamino]propan-1-ol수율 104%

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

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, 0.66 mmol), and stirred at room temperature overnight. A 2N-hydrogen chloride methanol solution (0.5 ml) was added to the mixture, and stirred at 50° C. for 3 hours. Triethylamine (0.64 ml) was then added to the reaction mixture, and concentrated under reduced pressure. The residue was purified by basic silica gel column chromatography (dichloromethane). The purified product was concentrated under reduced pressure to thereby obtain 186.3 mg (yield: quantitative) of 3-[(2-pyridin-3-ylethyl)pyridin-4-ylmethylamino]propan-1-ol as an orange oil.

후처리

  1. stirringstirred at 50° C. for 3 hours
  2. concentrationconcentrated under reduced pressure
  3. customThe residue was purified by basic silica gel column chromatography (dichloromethane)
  4. concentrationThe purified product was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-1f873d8bd3524e05b6835abaeef669e6
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08664217B2

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