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

HRID 1504167노트

반응식

HRID 1504167 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 103.4%

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). 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.

후처리

  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

출처 및 근거

ORD 기록
ord-63cfd05b3d2a438aa3ea1b4bc8778b70
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09212187B2

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