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Hydrochloric Acid → HCID 57976187, 화합물

HRID 420888
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HRID 420888 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9]=[O:10])=[CH:4][C:3]=1[C:11]([F:14])([F:13])[F:12].[NH2:15][C:16]([CH3:22])([CH2:20][OH:21])[C:17](O)=[O:18].Cl>O1CCOCC1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:17](=[O:18])[C:16]([CH2:20][OH:21])([CH3:22])[NH:15][C:9]2=[O:10])=[CH:4][C:3]=1[C:11]([F:12])([F:13])[F:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 943092-MethylserineHCID 27332651-Chloro-4-isocyanato-2-(trifluoromethyl) benzene

생성물 1

HCID 57976187HCID 57976187, 화합물수율 41.4%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

1-Chloro-4-isocyanato-2-trifluoromethyl-benzene (4.40 g, 20 mmoL) and 2-amino-3-hydroxy-2-methyl-propionic acid (2.38 g, 20 mmoL) in dioxane (100 mL) was heated at 80° C. for 6 hrs. The reaction was cooled to room temperature and concentrated HCl (2 mL) was added and the reaction mixture was heated to refluxed for 4 hrs. The solvent was removed and the residue was partitioned between ethyl acetate and water. The organic layer was washed with sat. NaHCO3, brine, dried over anhydrous Na2SO4, filtered and concentrated, then recrystallization was conducted using ethyl acetate as solvent to afford the title compound as a white solid (2.65 g, yield 41%).

후처리

  1. temperaturethe reaction mixture was heated
  2. temperatureto refluxed for 4 hrs
  3. customThe solvent was removed
  4. customthe residue was partitioned between ethyl acetate and water
  5. washThe organic layer was washed with sat. NaHCO3, brine
  6. dry with materialdried over anhydrous Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customrecrystallization

출처 및 근거

ORD 기록
ord-56ede8229dfe47b1a0b6cc376ab3643c
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08097730B2

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