Hydrochloric Acid → 1-(4-methylpiperidin-3-yl)-6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazine hydrochloride

HRID 2204565노트

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HRID 2204565 반응식
[C:1]1([CH:13]2[CH:18]([CH3:19])[CH2:17][CH2:16][N:15](C(OC(C)(C)C)=O)[CH2:14]2)[N:5]2[C:6]3[CH:12]=[CH:11][NH:10][C:7]=3[N:8]=[CH:9][C:4]2=[CH:3][N:2]=1.[ClH:27]>O1CCOCC1.CCOCC>[ClH:27].[CH3:19][CH:18]1[CH2:17][CH2:16][NH:15][CH2:14][CH:13]1[C:1]1[N:5]2[C:6]3[CH:12]=[CH:11][NH:10][C:7]=3[N:8]=[CH:9][C:4]2=[CH:3][N:2]=1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 58009929tert-butyl 3-(6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazin-1-yl)-4-methylpiperidine-1-carboxylate

생성물 1

HCID 670685881-(4-methylpiperidin-3-yl)-6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazine hydrochloride수율 99.9%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 312751,4-Dioxane용매

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온도
60 °C

실험 절차

To a solution of tert-butyl 3-(6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazin-1-yl)-4-methylpiperidine-1-carboxylate (12.2 g, 34.3 mmol) in 1,4-dioxane (100 mL) was added 4N HCl (4N in 1,4-dioxane, 25.7 mL, 103 mmol). The reaction mixture was heated at about 60° C. for about 2 h. The mixture was allowed to cool to ambient temperature and was diluted with Et2O (100 mL). The mixture was triturated and filtered, and the precipitate was washed with Et2O (100 mL) to give 1-(4-methylpiperidin-3-yl)-6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazine hydrochloride (10 g, 98% yield) as a tan solid: LC/MS (Table 2, Method a) Rt=1.05 min; MS m/z: 256 (M+H)+.

후처리

  1. temperatureto cool to ambient temperature
  2. customThe mixture was triturated
  3. filtrationfiltered
  4. washthe precipitate was washed with Et2O (100 mL)

출처 및 근거

ORD 기록
ord-8f6ffa91fe974d9b9615a1632d804e7c
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09365579B2

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