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

HRID 42178

反応式

HRID 42178 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-027bcfb2f02b474e89a07d6e5c810596
出典データセット
uspto-grants-2013_09
特許番号
US08536168B2

関連ノート

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