Carbonic acid sodium salt (1:2) → 1-Benzyl-4-((R)-3-methyl-piperazin-1-yl)-phthalazine

HRID 42177

反应方程式

HRID 42177 反应方程式
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

参与物

5

反应物 3

HCID 10340Carbonic acid sodium salt (1:2)HCID 64045661-苄基-4-氯酞嗪HCID 7330434(R)-(-)-2-甲基哌嗪

产物 1

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

试剂、催化剂与溶剂 1

HCID 312751,4-二氧六环溶剂

实验过程

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).

后处理

  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

来源与证据

ORD记录
ord-254f7c629db147839715ceb1129a9f43
来源数据集
uspto-grants-2013_09
专利号
US08536168B2

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