P-Anisidine → HCID 178492212、化合物

HRID 1462199ノート

反応式

HRID 1462199 の反応式
[O:1]1[CH2:6][C:5](=O)[NH:4][C:3](=[O:8])[NH:2]1.[CH3:9][O:10][C:11]1[CH:17]=[CH:16][C:14]([NH2:15])=[CH:13][CH:12]=1.C[Si](C)(C)N[Si](C)(C)C>S([O-])([O-])(=O)=O.[NH4+].[NH4+].O1CCOCC1>[CH3:9][O:10][C:11]1[CH:17]=[CH:16][C:14]([NH:15][C:5]2[CH2:6][O:1][NH:2][C:3](=[O:8])[N:4]=2)=[CH:13][CH:12]=1

参加物

6

反応物 3

HCID 7732P-AnisidineHCID 13838HexamethyldisilazaneHCID 642154HCID 642154、化合物

生成物 1

HCID 178492212HCID 178492212、化合物収率 59%

試薬・触媒・溶媒 2

HCID 6097028Ammonium Sulfate触媒HCID 312751,4-Dioxane溶媒

実験手順

A solution of 1.16 g (0.010 mole) of 6H-1,2,4-oxadiazin-3,5(2H,4H)-dione, 5 mg ammonium sulfate, 1.47 g (0.012 mole) of p-methoxyaniline and 20 ml hexamethyldisilazane in 40 ml of freshly distilled dry dioxane is refluxed for 17 hours. After cooling, the dioxane and hexamethyldisilazane are removed in vacuo and the syrupy residue is dried on a vacuum pump for 2 hours. The resulting semi-solid residue is triturated with 100 ml of petroleum ether and filtered to give a yield of 1.3 g (59 percent) of 5-((4-methoxyphenyl)amino)-6H-1,2,4-oxadiazin-3(2H)-one.

後処理

  1. temperatureis refluxed for 17 hours
  2. temperatureAfter cooling
  3. customthe dioxane and hexamethyldisilazane are removed in vacuo
  4. customthe syrupy residue is dried on a vacuum pump for 2 hours
  5. customThe resulting semi-solid residue is triturated with 100 ml of petroleum ether
  6. filtrationfiltered

出典と根拠

ORDレコード
ord-e4a9ec64bdfa495cb6bfa9a8bf30333b
出典データセット
uspto-grants-1984_07
特許番号
US04459403

反応ノート

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