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

HRID 2204565ノート

反応式

HRID 2204565 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
60 °C

実験手順

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)+.

後処理

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

出典と根拠

ORDレコード
ord-8f6ffa91fe974d9b9615a1632d804e7c
出典データセット
uspto-grants-2016_06
特許番号
US09365579B2

反応ノート

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