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Cesium carbonate → tert-butyl 3-(6-bromo-2-methyl-1H-benzo[d]imidazol-1-yl)azetidine-1-carboxylate

HRID 879533
ノート
印刷プレビュー

反応式

HRID 879533 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-])=O)=[C:4](F)[CH:3]=1.C([O-])([O-])=O.[Cs+].[Cs+].[NH2:18][CH:19]1[CH2:22][N:21]([C:23]([O:25][C:26]([CH3:29])([CH3:28])[CH3:27])=[O:24])[CH2:20]1.[CH3:30][C:31](OCC)(OCC)OCC>CN(C=O)C.CCOC(C)=O.O.CCO.CCOC(C)=O.CC(O)=O.[Pt]>[Br:1][C:2]1[CH:7]=[CH:6][C:5]2[N:8]=[C:30]([CH3:31])[N:18]([CH:19]3[CH2:20][N:21]([C:23]([O:25][C:26]([CH3:29])([CH3:28])[CH3:27])=[O:24])[CH2:22]3)[C:4]=2[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

11

反応物 4

HCID 10796Cesium carbonateHCID 66221Triethyl orthoacetateHCID 1516507Tert-butyl 3-aminoazetidine-1-carboxylateHCID 27833624-Bromo-2-fluoro-1-nitrobenzene

生成物 1

HCID 86700353tert-butyl 3-(6-bromo-2-methyl-1H-benzo[d]imidazol-1-yl)azetidine-1-carboxylate

試薬・触媒・溶媒 6

HCID 23939
Platinum
触媒
HCID 176Acetic Acid溶媒
HCID 962Water溶媒
HCID 6228Dimethylformamide溶媒
HCID 8857Ethyl Acetate溶媒
HCID 21584252Ethanol ethylacetate溶媒

実験手順

A flask was charged with 4-bromo-2-fluoro-1-nitrobenzene (529 mg, 2.41 mmol), Cs2CO3 (2.45 g, 7.52 mmol), and diluted with DMF (6 mL). To this was added tert-butyl 3-aminoazetidine-1-carboxylate (0.75 mL, 4.78 mmol) at room temperature and the reaction mixture was allowed to stir for 16 hours. The mixture was diluted with EtOAc and H2O and the layers were separated. The aqueous layer was extracted with EtOAc and the combined organic extracts were dried over Na2SO4, filtered through a small pad of silica gel eluting with 30% EtOAc/Hex, and concentrated in vacuo to afford a crude residue. The flask containing the crude residue was charged 5 wt % Pt/C (140 mg) and then diluted with 2:1 EtOH/EtOAc (30 mL). The flask was evacuated then backfilled with H2 (3 cycles) and stirred under a hydrogen atmosphere for 20 minutes, at which time, the flask was purged with N2, filtered through a pad of Celite, and concentrated in vacuo to provide a crude residue. The crude residue was taken up in AcOH (10 mL) and MeC(OEt)3 (1 mL) was added at room temperature, stirred for 15 minutes, and then the solution was concentrated in vacuo. The crude residue was purified by silica gel column chromatography (30-70% EtOAc/Hex gradient) to afford the desired product. LCMS-ESI+: calc'd C16H21BrN3O2: 366.1 (M+H+); Found: 366.1 (M+H+).

後処理

  1. customthe layers were separated
  2. extractionThe aqueous layer was extracted with EtOAc
  3. dry with materialthe combined organic extracts were dried over Na2SO4
  4. filtrationfiltered through a small pad of silica gel eluting with 30% EtOAc/Hex
  5. concentrationconcentrated in vacuo
  6. customto afford a crude residue
  7. customThe flask was evacuated
  8. stirringstirred under a hydrogen atmosphere for 20 minutes, at which time
  9. customthe flask was purged with N2
  10. filtrationfiltered through a pad of Celite
  11. concentrationconcentrated in vacuo
  12. customto provide a crude residue
  13. stirringstirred for 15 minutes
  14. concentrationthe solution was concentrated in vacuo
  15. customThe crude residue was purified by silica gel column chromatography (30-70% EtOAc/Hex gradient)

出典と根拠

ORDレコード
ord-a30cbefc534d41a886c54859485d089f
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08987250B2

反応ノート

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