Sodium Carbonate → 1-(2-(Piperazin-1-yl)pyrimidin-5-yl)ethanone hydrochloride

HRID 522676

反応式

HRID 522676 の反応式
[C:1]([C:4]1[CH:5]=[N:6][C:7]([N:10]2[CH2:15][CH2:14][N:13](C(OCCCC)=O)[CH2:12][CH2:11]2)=[N:8][CH:9]=1)(=[O:3])[CH3:2].C(OCC(F)(F)F)(=O)C.C(=O)([O-])[O-].[Na+].[Na+]>ClCCl>[N:10]1([C:7]2[N:6]=[CH:5][C:4]([C:1](=[O:3])[CH3:2])=[CH:9][N:8]=2)[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 1362562,2,2-Trifluoroethyl AcetateHCID 131735539Butyl 4-(5-acetylpyrimidin-2-yl)piperazine-1-carboxylate

生成物 1

HCID 1180224421-(2-(Piperazin-1-yl)pyrimidin-5-yl)ethanone hydrochloride収率 86%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of -butyl 4-(5-acetylpyrimidin-2-yl)piperazine-1-carboxylate (4.5 g, 14.7 mmol) in dichloromethane (80 mL) was added trifluoroethyl acetate (20 mL), and the mixture was stirred at RT for 3 h. LCMS showed the reaction was completed. The reaction mixture was neutralized with sodium carbonate solution and extracted with dichloromethane. The organic layer was dried over sodium sulfate, filtered and concentrated to afford the title compound as a light yellow solid (2.6 g, 86%), which was directly used in the next step without further purification. MS (ES+) C10H14N4O requires: 206, found: 207 [M+H]+.

後処理

  1. extractionextracted with dichloromethane
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-18eeb75877ba4bc0afdcd367ba7b7565
出典データセット
uspto-grants-2016_05
特許番号
US09334263B2

関連ノート

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