Water → HCID 23143330, 화합물

HRID 732178노트

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HRID 732178 반응식
[CH3:1][C:2]1[O:6][C:5](=O)[NH:4][C:3]=1[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.P(Cl)(Cl)([Cl:16])=O.N1C=CC=CC=1.O>C(#N)C>[Cl:16][C:5]1[O:6][C:2]([CH3:1])=[C:3]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:4]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 1049PyridineHCID 24813Phosphorus oxychlorideHCID 123070002(3H)-Oxazolone, 5-methyl-4-phenyl-

생성물 1

HCID 23143330HCID 23143330, 화합물수율 49.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
120 °C

실험 절차

To a suspension of 5-methyl-4-phenyl-1,3-oxazol-2(3H)-one (430 mg, 2.45 mmol) in phosphorus oxychloride (2.36 g, 14.7 mmol) was added pyridine (194 mg, 2.45 mmol) and the mixture was stirred at 120° C. for 2 hr. The reaction mixture was diluted with acetonitrile and added dropwise to water (about 30° C.). The organic materials were extracted with ethyl acetate, washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=7:3) to give the title compound (233 mg, yield 49%) as a yellow oil.

후처리

  1. extractionThe organic materials were extracted with ethyl acetate
  2. washwashed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=7:3)

출처 및 근거

ORD 기록
ord-d07c2186d94441beb2a75acc0f474251
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07585880B2

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