Hexamethyldisilazane → HCID 178498124, 화합물

HRID 1462198노트

반응식

HRID 1462198 반응식
[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

참가 물질

6

반응물 3

HCID 13838HexamethyldisilazaneHCID 642154HCID 642154, 화합물HCID 22600504HCID 22600504, 화합물

생성물 1

HCID 178498124HCID 178498124, 화합물수율 63%

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, 1.80 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.

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-4d18aff7e10745c08310f7075840f089
출처 데이터셋
uspto-grants-1984_07
특허 번호
US04459403

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