Triethylamine → N-(4-nitrobenzyl)trifluoroacetoamide

HRID 856657

반응식

HRID 856657 반응식
Cl.[N+:2]([C:5]1[CH:12]=[CH:11][C:8]([CH2:9][NH2:10])=[CH:7][CH:6]=1)([O-:4])=[O:3].C(N(CC)CC)C.C([O:23][CH2:24][C:25]([F:28])([F:27])[F:26])(=O)C>C(#N)C>[N+:2]([C:5]1[CH:6]=[CH:7][C:8]([CH2:9][NH:10][C:24](=[O:23])[C:25]([F:28])([F:27])[F:26])=[CH:11][CH:12]=1)([O-:4])=[O:3]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 1362562,2,2-Trifluoroethyl AcetateHCID 112524674-Nitrobenzylamine hydrochloride

생성물 1

HCID 14317262N-(4-nitrobenzyl)trifluoroacetoamide

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a suspension of 4-nitrobenzylamine hydrochloride (10.0 g) and triethylamine (22.2 ml) in acetonitrile (100 ml) was added trifluoroethyl acetate (12.6 ml) at room temperature and the mixture was stirred for 24 hours. The solvent was removed under reduced pressure, water was added to the mixture and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate and concentrated under reduced pressure. The precipitated crystals were collected by filtration. The crystals were washed with hexane, to give N-(4-nitrobenzyl)trifluoroacetoamide (12.79 g) as colorless crystals.

후처리

  1. customThe solvent was removed under reduced pressure, water
  2. additionwas added to the mixture
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. filtrationThe precipitated crystals were collected by filtration
  8. washThe crystals were washed with hexane

출처 및 근거

ORD 기록
ord-2b75692cde864675be581d7fbd123640
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07262185B2

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