Acetic Anhydride → HCID 178471861, 화합물

HRID 1584815노트

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HRID 1584815 반응식
[Br:1][C:2]1[C:15]([F:16])=[CH:14][C:5]([C:6]([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])=[O:7])=[C:4]([F:17])[C:3]=1[CH3:18].[C:19](OC(=O)C)(=O)[CH3:20].CO[CH:28](OC)[N:29]([CH3:31])C.C1(N)CC1>C(Cl)Cl.C(O)C.CCCCCC>[Br:1][C:2]1[C:15]([F:16])=[CH:14][C:5]([C:6]([C:8](=[CH:31][NH:29][CH:28]2[CH2:20][CH2:19]2)[C:9]([O:11][CH2:12][CH3:13])=[O:10])=[O:7])=[C:4]([F:17])[C:3]=1[CH3:18]

참가 물질

8

반응물 4

HCID 7918Acetic AnhydrideHCID 69828CyclopropylamineHCID 78373Dimethylformamide dimethyl acetalHCID 21220244Ethyl 4-bromo-2,5-difluoro-3-methylbenzoylacetate

생성물 1

HCID 178471861HCID 178471861, 화합물

시약·촉매·용매 3

HCID 702Ethanol용매HCID 6344Dichloromethane용매HCID 8058Hexane용매

실험 절차

In 150 ml of methylene chloride was dissolved 30.0 g of ethyl 4-bromo-2,5-difluoro-3-methylbenzoylacetate, and 19.1 g of acetic anhydride and 22.3 g of N,N-dimethylformamide dimethyl acetal were added to the solution, after which the resulting mixture was stirred at room temperature for one hour. Thereafter, the solvent was removed by distillation under reduced pressure. The residue obtained was dissolved in 90 ml of ethanol and 5.90 g of cyclopropylamine was added thereto, after which the resulting mixture was stirred at room temperature for 30 minutes. The solvent was then removed by distillation under reduced pressure. To the residue obtained was added n-hexane and the crystals formed were collected by filtration, to obtain 35.7 g of colorless, crystalline ethyl 2-(4-bromo-2,5-difluoro-3-methylbenzoyl)-3-cyclopropylaminoacrylate.

후처리

  1. additionwere added to the solution
  2. customThereafter, the solvent was removed by distillation under reduced pressure
  3. customThe residue obtained
  4. stirringafter which the resulting mixture was stirred at room temperature for 30 minutes
  5. customThe solvent was then removed by distillation under reduced pressure
  6. customTo the residue obtained
  7. customthe crystals formed
  8. filtrationwere collected by filtration

출처 및 근거

ORD 기록
ord-da6ad9c6b29049c28b13c1b9c483af8a
출처 데이터셋
uspto-grants-1999_08
특허 번호
US05935952

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