Dodecylamine → HCID 178443234、化合物

HRID 1462193ノート

反応式

HRID 1462193 の反応式
[O:1]1[CH2:6][C:5](=O)[NH:4][C:3](=[O:8])[NH:2]1.[CH2:9]([NH2:21])[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20].C[Si](C)(C)N[Si](C)(C)C>S([O-])([O-])(=O)=O.[NH4+].[NH4+].O1CCOCC1>[CH2:9]([NH:21][C:5]1[CH2:6][O:1][NH:2][C:3](=[O:8])[N:4]=1)[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20]

参加物

6

反応物 3

HCID 13583DodecylamineHCID 13838HexamethyldisilazaneHCID 642154HCID 642154、化合物

生成物 1

HCID 178443234HCID 178443234、化合物収率 88.2%

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 of ammonium sulfate, 2.22 g (0.012 mole) of dodecylamine and 20 ml of 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 yield 2.5 g (88 percent) of 5-dodecylamino-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-9b28039e4f8a42f0b5600e820e311307
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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