Potassium Carbonate → HCID 59581200、化合物

HRID 1754062ノート

反応式

HRID 1754062 の反応式
Br[C:2]1[C:11]([Br:12])=[CH:10][C:5]2[O:6][CH2:7][CH2:8][O:9][C:4]=2[CH:3]=1.[C:13]([Cu])#[N:14].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[Br:12][C:11]1[C:2]([C:13]#[N:14])=[CH:3][C:4]2[O:9][CH2:8][CH2:7][O:6][C:5]=2[CH:10]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 27545026,7-Dibromobenzo(1,4)dioxanHCID 178418546HCID 178418546、化合物

生成物 1

HCID 59581200HCID 59581200、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
150 °C

実験手順

A mixture of 20.0 g (62.6 mmol) of 6,7-dibromo-2,3-dihydrobenzo[1,4]dioxine, 8.50 g (93.9 mmol) CuCN and 13.0 (93.9 mmol) K2CO3 in 300 mL DMF is stirred at 150° C. for 6 d. The reaction is quenched by the addition of water and extracted with EtOAc. The org. layers are combined and washed with water (3×) and sat. aq. NaCl solution. After drying over Na2SO4, the mixture is filtered and the solvent is removed in vacuo. The resulting residue is purified by column chromatography (silica gel, PE/EtOAc 20/1→10/1).

後処理

  1. customThe reaction is quenched by the addition of water
  2. extractionextracted with EtOAc
  3. washwashed with water (3×) and sat. aq. NaCl solution
  4. dry with materialAfter drying over Na2SO4
  5. filtrationthe mixture is filtered
  6. customthe solvent is removed in vacuo
  7. customThe resulting residue is purified by column chromatography (silica gel, PE/EtOAc 20/1→10/1)

出典と根拠

ORDレコード
ord-d7fc5e04cc1e429bb5396ec9eaa4d9b7
出典データセット
uspto-grants-2015_10
特許番号
US09169205B2

反応ノート

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