2-Hydrazinopyridine → 8-Methoxy-10,10-dimethyl-10,11-dihydro-5H-1,11-diaza-benzo[B]fluorene

HRID 2275170

反応式

HRID 2275170 の反応式
[NH:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1)N.[CH3:9][O:10][C:11]1[CH:20]=[C:19]2[C:14]([CH2:15][CH2:16][C:17](=O)[C:18]2([CH3:22])[CH3:21])=[CH:13][CH:12]=1>CN1C(=O)CCC1.C(OCC)(=O)C>[CH3:9][O:10][C:11]1[CH:12]=[CH:13][C:14]2[CH2:15][C:16]3[C:8]4[CH:7]=[CH:6][CH:5]=[N:4][C:3]=4[NH:1][C:17]=3[C:18]([CH3:21])([CH3:22])[C:19]=2[CH:20]=1

参加物

5

反応物 2

HCID 786452-HydrazinopyridineHCID 130110077-Methoxy-1,1-dimethyl-3,4-dihydronaphthalen-2(1H)-one2 回

生成物 1

HCID 668339058-Methoxy-10,10-dimethyl-10,11-dihydro-5H-1,11-diaza-benzo[B]fluorene

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
190 °C

実験手順

2-Hydrazinopyridine (1.3 g, 11.8 mmol) and 7-methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one (Compound A2, 2.4 g, 11.8 mmol) were dissolved in NMP (60 mL), and stirred at 190° C. for 48 hr. The reaction solution was diluted with ethyl acetate, washed with water and dried over magnesium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (hexane/ethyl acetate) to obtain the target compound (white solid, 101 mg, 3%).

後処理

  1. washwashed with water
  2. dry with materialdried over magnesium sulfate
  3. customThe drying agent was removed by filtration
  4. customthe residues obtained
  5. concentrationafter concentration under reduced pressure
  6. customwere purified by silica gel column chromatography (hexane/ethyl acetate)
  7. customto obtain the target compound (white solid, 101 mg, 3%)

出典と根拠

ORDレコード
ord-f450413031a54dcab8306c9bf4370fa1
出典データセット
uspto-grants-2015_09
特許番号
US09126931B2

関連ノート

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