Potassium Carbonate → HCID 15023616、化合物

HRID 973952

反応式

HRID 973952 の反応式
Cl.[N:2]1[CH:7]=[CH:6][C:5]([CH2:8]Cl)=[CH:4][CH:3]=1.[CH3:10][C:11]1([CH3:17])[CH2:15][O:14][NH:13][C:12]1=[O:16].C(=O)([O-])[O-].[K+].[K+].C1OCCOCCOCCOCCOCCOC1>C(#N)C.C(OCC)(=O)C>[CH3:10][C:11]1([CH3:17])[CH2:15][O:14][N:13]([CH2:8][C:5]2[CH:6]=[CH:7][N:2]=[CH:3][CH:4]=2)[C:12]1=[O:16]

参加物

7

反応物 4

HCID 11430Potassium CarbonateHCID 2855718-Crown-6HCID 745704-(Chloromethyl)pyridinium chlorideHCID 6421514,4-Dimethyl-1,2-oxazolidin-3-one

生成物 1

HCID 15023616HCID 15023616、化合物

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 4-picolyl chloride hydrochloride (1.4 g, 0.0084 mol), 4,4-dimethyl-3-isoxazolidinone (1.0 g, 0.0084 mol), potassium carbonate (3.6 g, 0.0261 mol), and 18-Crown-6 (0.10 g, 0.0004 mol) in acetonitrile (50 mL) is stirred at room temperature overnight. The reaction mixture is poured into ethyl acetate (50 mL) and the mixture washed with water (3×30 mL). The organic layer is dried (magnesium sulfate) and concentrated under reduced pressure to yield an oil. This oil is passed through a silica gel pad eluting with 4:1 chloroform:methanol. The filtrate is concentrated and converted to 1.4 g of the maleate salt of the title compound.

後処理

  1. washthe mixture washed with water (3×30 mL)
  2. dry with materialThe organic layer is dried (magnesium sulfate)
  3. concentrationconcentrated under reduced pressure
  4. customto yield an oil
  5. washeluting with 4:1 chloroform
  6. concentrationThe filtrate is concentrated

出典と根拠

ORDレコード
ord-8e261a37270e495a93f4a1dcd3cb1ad9
出典データセット
uspto-grants-1991_11
特許番号
US05066665

関連ノート

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