Hydrochloric Acid → 5-Bromo-1,3-dihydro-1,3-dimethyl-2H-benzimidazol-2-one

HRID 2386783ノート

反応式

HRID 2386783 の反応式
IC.[Br:3][C:4]1[CH:13]=[CH:12]C2N[C:9](=O)[NH:10][C:6]=2[CH:5]=1.CC(C)([O-])C.[K+].Cl.C[C:22]([N:24]([CH3:26])[CH3:25])=[O:23]>>[Br:3][C:4]1[CH:13]=[CH:12][C:25]2[N:24]([CH3:26])[C:22](=[O:23])[N:10]([CH3:9])[C:6]=2[CH:5]=1

参加物

6

反応物 5

HCID 313Hydrochloric AcidHCID 6328Methyl iodideHCID 31374DimethylacetamideHCID 122280605-Bromo-1,3-dihydro-2H-benzimidazol-2-oneHCID 23665647Potassium tert-butoxide

生成物 1

HCID 470034475-Bromo-1,3-dihydro-1,3-dimethyl-2H-benzimidazol-2-one

実験手順

Iodomethane (2.41 g) was added to a suspension of 5-bromo-1,3-dihydro-benzoimidazol-2-one (1.65 g) and potassium tert-butoxide (1.91 g) in DMA (20 ml). The mixture was stirred overnight at room temperature. The mixture was poured to 2.5N aqueous HCl (80 ml) and extracted with EtOAc. The combined organic layers were dried over Na2SO4 and then concentrated in vacuo. Heptane (50 ml) was added to the residue and the mixture was filtered. The residue was washed with diethyl ether and dried in vacuo to give the title compound (1.1 g) as a light brown solid. MS (m/e)=241.1 [M+H+].

後処理

  1. extractionextracted with EtOAc
  2. dry with materialThe combined organic layers were dried over Na2SO4
  3. concentrationconcentrated in vacuo
  4. additionHeptane (50 ml) was added to the residue
  5. filtrationthe mixture was filtered
  6. washThe residue was washed with diethyl ether
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-fee2e925739c48ef8a0c41283ff96c9f
出典データセット
uspto-grants-2012_09
特許番号
US08268820B2

反応ノート

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