(1-methylpiperidin-4-yl)(pyridin-2-yl)methanone → HCID 131727019, 화합물

HRID 404244노트

반응식

HRID 404244 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]([C:8]([C:10]2[N:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[O:9])[CH2:4][CH2:3]1.[ClH:16].C(O)C>C(O)C>[ClH:16].[ClH:16].[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]([C:8]([C:10]2[N:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[O:9])[CH2:4][CH2:3]1

참가 물질

4

반응물 2

HCID 11321671(1-methylpiperidin-4-yl)(pyridin-2-yl)methanoneHCID 21887872Ethanol hydrochloride

생성물 1

HCID 131727019HCID 131727019, 화합물수율 63%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Resuspend the crude 2-amino-(6-(1-methylpiperidin-4-ylcarbonyl)-pyridine (14.5 g, 66.2 mmol) in ethanol (30 mL), add 2.5M HCl/ethanol (100 mL), stir the mixture for 30 minutes, and then remove the solvent under reduce pressure. Resuspend the resulting solid in 125 ml isopropanol and heat under reflux for 30 minutes. Cool the reaction mixture to room temperature, filtered-off the precipitate, rinse with 20 ml isopropanol, and dry under vacuum at 50° C. to obtain 2-amino-(6-(1-methylpiperidin-4-ylcarbonyl)-pyridine 2HCl (11 g, 63% yield corrected by HPLC % w/w).

후처리

  1. customremove the solvent
  2. temperatureheat
  3. temperatureunder reflux for 30 minutes
  4. washfiltered-off the precipitate, rinse with 20 ml isopropanol
  5. customdry under vacuum at 50° C.

출처 및 근거

ORD 기록
ord-352b98cc756f418bb3de526a254e0c42
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08748459B2

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