Piperazine → 4-Chloro-5-methoxy-6-(piperazin-1-yl)pyrimidine

HRID 591143

반응식

HRID 591143 반응식
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[Cl:7][C:8]1[C:13]([O:14][CH3:15])=[C:12](Cl)[N:11]=[CH:10][N:9]=1>O>[Cl:7][C:8]1[C:13]([O:14][CH3:15])=[C:12]([N:1]2[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]2)[N:11]=[CH:10][N:9]=1

참가 물질

4

반응물 2

HCID 4837PiperazineHCID 787204,6-Dichloro-5-methoxypyrimidine2회

생성물 1

HCID 150205444-Chloro-5-methoxy-6-(piperazin-1-yl)pyrimidine수율 103.9%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Piperazine (6.00 g, 70 mmol, 6.25 eq) is dissolved in water (30 ml), and to this solution is added 4,6-dichloro-5-methoxypyrimidine (2.00 g, 11.2 mmol, 1.0 eq). The mixture is stirred vigorously at room temperature for 2.0 h, during which 4,6-dichloro-5-methoxypyrimidine is gradually dissolved. The aqueous phase is extracted with CH2Cl2 (25 ml*2). The extracted liquids are combined, dried over anhydrous sodium sulfate and filtered by vacuum filtration, and concentrated to give a light yellow oily crude product (2.66 g).

후처리

  1. dissolutionis gradually dissolved
  2. extractionThe aqueous phase is extracted with CH2Cl2 (25 ml*2)
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltered by vacuum filtration
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8457e706421a47fab48a915dfdd7b939
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09238632B2

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