Hexamethyldisilazane → HCID 178498124、化合物

HRID 1462198ノート

反応式

HRID 1462198 の反応式
[O:1]1[CH2:6][C:5](=O)[NH:4][C:3](=[O:8])[NH:2]1.[NH2:9][C:10]1[CH:18]=[CH:17][C:13]([C:14]([O-:16])=[O:15])=[C:12](C)[CH:11]=1.[CH3:20][Si](C)(C)N[Si](C)(C)C>S([O-])([O-])(=O)=O.[NH4+].[NH4+].O1CCOCC1>[O:8]=[C:3]1[N:4]=[C:5]([NH:9][C:10]2[CH:18]=[CH:17][C:13]([C:14]([O:16][CH3:20])=[O:15])=[CH:12][CH:11]=2)[CH2:6][O:1][NH:2]1

参加物

6

反応物 3

HCID 13838HexamethyldisilazaneHCID 642154HCID 642154、化合物HCID 22600504HCID 22600504、化合物

生成物 1

HCID 178498124HCID 178498124、化合物収率 63%

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, 1.80 g (0.012 mole) of p-amino-methylbenzoate and 20 ml hexamethyldisilazane in 40 ml 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 yield 1.56 g (63 percent) of 4-((3,6-dihydro-3-oxo-2H-1,2,4-oxadiazin-5-yl)amino)benzoic acid, methyl ester.

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-4d18aff7e10745c08310f7075840f089
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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