Potassium Carbonate → 4-(1,4-diazabicyclo[3.2.2]nonan-4-yl)-N-methyl-2-nitrobenzamide

HRID 77381

反応式

HRID 77381 の反応式
F[C:2]1[CH:11]=[CH:10][C:5]([C:6]([NH:8][CH3:9])=[O:7])=[C:4]([N+:12]([O-:14])=[O:13])[CH:3]=1.[N:15]12[CH2:23][CH2:22][CH:19]([CH2:20][CH2:21]1)[NH:18][CH2:17][CH2:16]2.C(=O)([O-])[O-].[K+].[K+]>CS(C)=O>[N:15]12[CH2:23][CH2:22][CH:19]([CH2:20][CH2:21]1)[N:18]([C:2]1[CH:11]=[CH:10][C:5]([C:6]([NH:8][CH3:9])=[O:7])=[C:4]([N+:12]([O-:14])=[O:13])[CH:3]=1)[CH2:17][CH2:16]2

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 3984071,4-Diazabicyclo(3.2.2)nonaneHCID 671150044-fluoro-N-methyl-2-nitrobenzamide2 回

生成物 1

HCID 671150264-(1,4-diazabicyclo[3.2.2]nonan-4-yl)-N-methyl-2-nitrobenzamide収率 81.8%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
90 °C

実験手順

To a solution of 4-fluoro-N-methyl-2-nitrobenzamide (Intermediate 3L) (0.65 g, 3.3 mmol) in dimethylsulfoxide (50 mL) was added 1,4-diazabicyclo[3.2.2]nonane (0.62 g, 4.9 mmol) and potassium carbonate (1.36 g, 9.8 mmol). The resulting suspension was heated at 90° C. for 4 days. The mixture was filtered and the filtrate purified using a 20 g SCX cartridge to afford 4-(1,4-diazabicyclo[3.2.2]nonan-4-yl)-N-methyl-2-nitrobenzamide (0.8 g, 2.7 mmol).

後処理

  1. filtrationThe mixture was filtered
  2. customthe filtrate purified

出典と根拠

ORDレコード
ord-3f89614c27bc483b8a741ea5d3ee1480
出典データセット
uspto-grants-2014_09
特許番号
US08841289B2

関連ノート

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