Cesium carbonate → HCID 57426193、化合物

HRID 551027ノート

反応式

HRID 551027 の反応式
C(=O)([O-])[O-].[Cs+].[Cs+].[N+:7]([C:10]1[C:18]2[NH:17][C:16](=[O:19])[NH:15][C:14]=2[CH:13]=[CH:12][CH:11]=1)([O-:9])=[O:8].Br[CH2:21][C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23]>>[N+:7]([C:10]1[C:18]2[NH:17][C:16](=[O:19])[N:15]([CH2:21][C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23])[C:14]=2[CH:13]=[CH:12][CH:11]=1)([O-:9])=[O:8]

参加物

4

反応物 3

HCID 10796Cesium carbonateHCID 79177tert-Butyl bromoacetateHCID 41498284-Nitro-1H-benzo[d]imidazol-2(3H)-one2 回

生成物 1

HCID 57426193HCID 57426193、化合物

実験手順

Cesium carbonate (1.75 g, 5.4 mmol) was added to a solution of 4-nitro-1,3-dihydro-2H-benzimidazol-2-one (800 mg, 4.5 mmol, described in Intermediate 26) and tert-butyl bromoacetate (0.791 mL, 5.4 mmol) in DM (15 mL). After 18 h, the reaction was quenched with H2O (100 mL) and the solid precipitate was collected by filtration. The crude product was purified by silica gel chromatography, eluting with CH2Cl2:MeOH—95:5, to give the title compound. MS: m/z=294 (M+1).

後処理

  1. customthe reaction was quenched with H2O (100 mL)
  2. filtrationthe solid precipitate was collected by filtration
  3. customThe crude product was purified by silica gel chromatography
  4. washeluting with CH2Cl2

出典と根拠

ORDレコード
ord-a0c1a45ebade4fae81459ac08093e97d
出典データセット
uspto-grants-2011_05
特許番号
US07947677B2

反応ノート

読み込み中…