Potassium Carbonate → 3-(4-Bromo-3,5-dimethylphenoxy)-1-methylpyrrolidin-2-one

HRID 237552ノート

反応式

HRID 237552 の反応式
[Br:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([OH:9])=[CH:4][C:3]=1[CH3:10].Br[CH:12]1[CH2:16][CH2:15][N:14]([CH3:17])[C:13]1=[O:18].C([O-])([O-])=O.[K+].[K+]>CN(C)C=O>[Br:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([O:9][CH:12]2[CH2:16][CH2:15][N:14]([CH3:17])[C:13]2=[O:18])=[CH:4][C:3]=1[CH3:10]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 819704-Bromo-3,5-dimethylphenolHCID 111829543-Bromo-1-methylpyrrolidin-2-one

生成物 1

HCID 866972183-(4-Bromo-3,5-dimethylphenoxy)-1-methylpyrrolidin-2-one

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 4-bromo-3,5-dimethylphenol (100 mg) in N,N-dimethylformamide (2 mL) is added 3-bromo-1-methylpyrrolidin-2-one (100 mg) and K2CO3 (105 mg). The mixture is stirred for 12 hours at room temperature. Then the mixture is partitioned between water and diethylether. The organic phase is dried (MgSO4) and concentrated. The residue is chromatographed on silica gel (cyclohexane/ethyl acetate 80:20→50:50) to give the title compound. Yield: 65 mg; LC (method 7): tR=1.0 min; Mass spectrum (ESI+): m/z=298 [M+H]+.

後処理

  1. customThen the mixture is partitioned between water and diethylether
  2. dry with materialThe organic phase is dried (MgSO4)
  3. concentrationconcentrated
  4. customThe residue is chromatographed on silica gel (cyclohexane/ethyl acetate 80:20→50:50)

出典と根拠

ORDレコード
ord-e9e8c9c3040d4ed78c35abd9e13ca709
出典データセット
uspto-grants-2014_02
特許番号
US08642585B2

反応ノート

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