Ammonium Chloride → HCID 86705193、化合物

HRID 2401286ノート

反応式

HRID 2401286 の反応式
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]

参加物

7

反応物 3

HCID 25517Ammonium ChlorideHCID 86705191HCID 86705191、化合物HCID 178455851HCID 178455851、化合物

生成物 1

HCID 86705193HCID 86705193、化合物

試薬・触媒・溶媒 3

HCID 53384555HCID 53384555、化合物触媒HCID 8028Tetrahydrofuran溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-68a84c6d3c244c0ca6bf3e0f99a64dd5
出典データセット
uspto-grants-2014_08
特許番号
US08796272B2

反応ノート

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