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

HRID 522676

반응식

HRID 522676 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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]+.

후처리

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

출처 및 근거

ORD 기록
ord-18eeb75877ba4bc0afdcd367ba7b7565
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09334263B2

연결된 노트

불러오는 중…