Water → 1-Benzyl-4-[4-(4-nitro-phenyl)-piperidine-1-yl]-phthalazine

HRID 42184

反応式

HRID 42184 の反応式
[CH2:1]([C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:11](Cl)=[N:10][N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N+:19]([C:22]1[CH:27]=[CH:26][C:25]([CH:28]2[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]2)=[CH:24][CH:23]=1)([O-:21])=[O:20].O>CN1C(=O)CCC1>[CH2:1]([C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:11]([N:31]2[CH2:30][CH2:29][CH:28]([C:25]3[CH:26]=[CH:27][C:22]([N+:19]([O-:21])=[O:20])=[CH:23][CH:24]=3)[CH2:33][CH2:32]2)=[N:10][N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 962WaterHCID 64045661-Benzyl-4-chlorophthalazineHCID 159258174-(4-Nitrophenyl)piperidine

生成物 1

HCID 592405681-Benzyl-4-[4-(4-nitro-phenyl)-piperidine-1-yl]-phthalazine収率 81.6%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
150 °C

実験手順

To a solution of 1-benzyl-4-chloro-phthalazine (1.08 g, 4.04 mmol) in 8 mL NMP is added 4-(4-nitro-phenyl)piperidine (1 g, 4.85 mmol), TEA (1.68 mL, 12.12 mmol). The reaction mixture was heated to 150° C. for 45 min in a microwave reactor. Water was added to the reaction mixture to form a precipitate and the solid is collected by filtration and dried under vacuum. The resulting solid is purified by HPLC with acetonitril in water (from 20% to 100% with 3% 1-propanol) at 220 nm wavelength detection to provide the title compound (1.4 g, 78%).

後処理

  1. customto form a precipitate
  2. filtrationthe solid is collected by filtration
  3. customdried under vacuum
  4. customThe resulting solid is purified by HPLC with acetonitril in water (from 20% to 100% with 3% 1-propanol) at 220 nm wavelength detection

出典と根拠

ORDレコード
ord-74ca62b13cd84576afb3e3deb18b2930
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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