P-Anisidine → HCID 178492212, 화합물

HRID 1462199노트

반응식

HRID 1462199 반응식
[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

참가 물질

6

반응물 3

HCID 7732P-AnisidineHCID 13838HexamethyldisilazaneHCID 642154HCID 642154, 화합물

생성물 1

HCID 178492212HCID 178492212, 화합물수율 59%

시약·촉매·용매 2

HCID 6097028Ammonium Sulfate촉매HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e4a9ec64bdfa495cb6bfa9a8bf30333b
출처 데이터셋
uspto-grants-1984_07
특허 번호
US04459403

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