Hydrochloric Acid → HCID 59309885, 화합물

HRID 1513000

반응식

HRID 1513000 반응식
[F:1][C:2]1[C:3]([N:24]2[C:32](=[O:33])[C:31]3[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=3)[C:25]2=[O:34])=[CH:4][C:5]([S:10]([N:13]2[C:19]3[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=3[CH2:17][CH2:16][CH2:15][CH2:14]2)(=[O:12])=[O:11])=[C:6]([O:8]C)[CH:7]=1.B(Br)(Br)Br.Cl>C(Cl)Cl>[F:1][C:2]1[C:3]([N:24]2[C:25](=[O:34])[C:26]3[C:31](=[CH:30][CH:29]=[CH:28][CH:27]=3)[C:32]2=[O:33])=[CH:4][C:5]([S:10]([N:13]2[C:19]3[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=3[CH2:17][CH2:16][CH2:15][CH2:14]2)(=[O:11])=[O:12])=[C:6]([OH:8])[CH:7]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 25134Boron tribromideHCID 685144615-fluoro-2-(2,3,4,5-tetrahydro-1H-1-benzoazepin-1-ylsulfonyl)-4-(1,3-dioxo-1,3-dihydroisoindol-2-yl)anisole

생성물 1

HCID 59309885HCID 59309885, 화합물수율 83.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 5-fluoro-2-(2,3,4,5-tetrahydro-1H-1-benzoazepin-1-yl-sulfonyl)-4-(1,3-dioxo-1,3-dihydroisoindol-2-yl)anisole (0.57 g) in methylene chloride (12 mL) was added boron tribromide (1 mol/L methylene chloride solution, 3.53 mL) under ice-cooling, and the mixture was stirred at room temperature for 3 hours. To the reaction mixture was added 1 mol/L hydrochloric acid, and the resulting mixture was extracted with ethyl acetate. The extract was washed with brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the residue was purified by column chromatography on silica gel (eluent: n-hexane−n-hexane/ethyl acetate=1/1) to give the title compound (0.46 g).

후처리

  1. temperaturecooling
  2. extractionthe resulting mixture was extracted with ethyl acetate
  3. washThe extract was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customthe residue was purified by column chromatography on silica gel (eluent: n-hexane−n-hexane/ethyl acetate=1/1)

출처 및 근거

ORD 기록
ord-3a39546a4deb4d2b99fdfd16e6175a62
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08217069B2

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