Ammonium Chloride → HCID 86705193, 화합물

HRID 2401286노트

반응식

HRID 2401286 반응식
Br[C:2]1[N:7]=[CH:6][C:5]([N:8]2[CH2:12][C@H:11]([CH:13]([CH3:15])[CH3:14])[N:10]([CH2:16][C:17]([NH:19][C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([C:26]([F:29])([F:28])[F:27])[CH:21]=3)=[O:18])[C:9]2=[O:30])=[CH:4][CH:3]=1.[CH2:31]([Mg]Br)[CH2:32][CH3:33].[Cl-].[NH4+]>C1COCC1.CN1C(=O)CCC1.C/C(/[O-])=C\C(C)=O.C/C(/[O-])=C\C(C)=O.C/C(/[O-])=C\C(C)=O.[Fe+3]>[O:30]=[C:9]1[N:8]([C:5]2[CH:6]=[N:7][C:2]([CH2:31][CH2:32][CH3:33])=[CH:3][CH:4]=2)[CH2:12][C@H:11]([CH:13]([CH3:15])[CH3:14])[N:10]1[CH2:16][C:17]([NH:19][C:20]1[CH:25]=[CH:24][CH:23]=[C:22]([C:26]([F:29])([F:28])[F:27])[CH:21]=1)=[O:18]

참가 물질

7

반응물 3

HCID 25517Ammonium ChlorideHCID 86705191HCID 86705191, 화합물HCID 178455851HCID 178455851, 화합물

생성물 1

HCID 86705193HCID 86705193, 화합물

시약·촉매·용매 3

HCID 53384555HCID 53384555, 화합물촉매HCID 8028Tetrahydrofuran용매HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

To a suspension of 2-[(5S)-3-(6-bromopyridin-3-yl)-2-oxo-5-(propan-2-yl)imidazolidin-1-yl]-N-[3-(trifluoromethyl)phenyl]acetamide (50 mg) and tris(2,4-pentanedionato)iron(III) (55 mg) in THF (1 mL) and NMP (0.1 mL) was added n-propylmagnesium bromide (2M solution in THF, 0.31 mL), and the mixture was stirred at room temperature for 1 hr. Saturated aqueous ammonium chloride solution was added thereto, the resulting mixture was extracted with acetic acid, and the organic layer was washed with water and brine. After drying over anhydrous sodium sulfate, the desiccant was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography (hexane/ethyl acetate) to afford the title compound (24 mg).

후처리

  1. extractionthe resulting mixture was extracted with acetic acid
  2. washthe organic layer was washed with water and brine
  3. dry with materialAfter drying over anhydrous sodium sulfate
  4. filtrationthe desiccant was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customThe residue was purified by column chromatography (hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-68a84c6d3c244c0ca6bf3e0f99a64dd5
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08796272B2

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