Sodium Carbonate → 1-benzyl-4-((S)-3-methyl-piperazin-1-yl)-phthalazine

HRID 42178

반응식

HRID 42178 반응식
C([O-])([O-])=O.[Na+].[Na+].[CH2:7]([C:14]1[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[C:17](Cl)=[N:16][N:15]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[CH3:25][C@H:26]1[CH2:31][NH:30][CH2:29][CH2:28][NH:27]1>O1CCOCC1>[CH2:7]([C:14]1[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[C:17]([N:30]2[CH2:29][CH2:28][NH:27][C@@H:26]([CH3:25])[CH2:31]2)=[N:16][N:15]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 27342192-Methylpiperazine, (S)-HCID 64045661-Benzyl-4-chlorophthalazine

생성물 1

HCID 441864791-benzyl-4-((S)-3-methyl-piperazin-1-yl)-phthalazine수율 64.1%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
100 °C

실험 절차

Solid Na2CO3 (400 mg, 3.8 mmol, 3.8 eq) is added to a solution of 1-benzyl-4-chlorophthalazine (250 mg, 0.98 mmol, 1 eq) and (5)-2-methyl-piperazine (400 mg, 4.0 mmol, 4.0 eq) in dioxane (5 mL). The resulting suspension is heated at 100° C. for 48 h. The reaction mixture is concentrated, EtOAc (50 mL) and water (15 mL) are added. The organic fraction washed with water and then brine, then is dried over sodium sulfate. The solvent is evaporated under reduced pressure to afford the title compound as a white solid (200 mg, 64% yield).

후처리

  1. concentrationThe reaction mixture is concentrated
  2. additionEtOAc (50 mL) and water (15 mL) are added
  3. washThe organic fraction washed with water
  4. dry with materialbrine, then is dried over sodium sulfate
  5. customThe solvent is evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-027bcfb2f02b474e89a07d6e5c810596
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536168B2

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