Sodium Carbonate → 1-Benzyl-4-((R)-3-methyl-piperazin-1-yl)-phthalazine

HRID 42177

반응식

HRID 42177 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 64045661-Benzyl-4-chlorophthalazineHCID 73304342-Methylpiperazine, (R)-

생성물 1

HCID 441862481-Benzyl-4-((R)-3-methyl-piperazin-1-yl)-phthalazine수율 58%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

Solid Na2CO3 (200 mg, 1.9 mmol, 1.9 eq) is added to a solution of 1-benzyl-4-chlorophthalazine (250 mg, 0.98 mmol, 1 eq) and (R)-2-methyl-piperazine (400 mg, 4.0 mmol, 4.0 eq) in dioxane (5 mL) in a microwave vial. The vial is sealed and irradiated in the microwave at 150° C. (high absorption setting) for 30 minutes. The reaction mixture is filtered and concentrated, then diluted with EtOAc (50 mL) and water (15 mL). 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 (180 mg, 58% yield).

후처리

  1. customThe vial is sealed
  2. customirradiated in the microwave at 150° C. (high absorption setting) for 30 minutes
  3. filtrationThe reaction mixture is filtered
  4. concentrationconcentrated
  5. additiondiluted with EtOAc (50 mL) and water (15 mL)
  6. washThe organic fraction washed with water
  7. dry with materialbrine, then is dried over sodium sulfate
  8. customThe solvent is evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-254f7c629db147839715ceb1129a9f43
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536168B2

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