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Water → 5-methyl-4-phenyl-2-(trifluoromethyl)-6H-1,3-oxazine-6-one

HRID 1650708
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HRID 1650708 반응식
[CH3:1][C:2](=[C:6]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[NH:7][C:8](=[O:13])[C:9]([F:12])([F:11])[F:10])[C:3](O)=[O:4].O>C(OC(=O)C)(=O)C>[CH3:1][C:2]1[C:3](=[O:4])[O:13][C:8]([C:9]([F:12])([F:11])[F:10])=[N:7][C:6]=1[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 962WaterHCID 53712489HCID 53712489, 화합물

생성물 1

HCID 142804195-methyl-4-phenyl-2-(trifluoromethyl)-6H-1,3-oxazine-6-one수율 92.6%

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매2회

실험 절차

39.3 g of the product of Step B were refluxed in 80 ml of acetic anhydride and maintained at this temperature for 30 minutes and then allowed to cool. The acetic anhydride was expelled under reduced pressure and iced water was added to the residue. The precipitate obtained was separated, washed abundantly with water and then dissolved in ether. The organic solution was dried and concentrated to dryness under reduced pressure to obtain 34 g of the expected product melting at 70° C.

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후처리

  1. temperaturemaintained at this temperature for 30 minutes
  2. temperatureto cool
  3. additionwas added to the residue
  4. customThe precipitate obtained
  5. customwas separated
  6. washwashed abundantly with water
  7. dissolutiondissolved in ether
  8. customThe organic solution was dried
  9. concentrationconcentrated to dryness under reduced pressure

출처 및 근거

ORD 기록
ord-f763b23612214616989f99fe7e470545
출처 데이터셋
uspto-grants-1990_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04925859

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