Potassium Carbonate → HCID 59581200, 화합물

HRID 1754062노트

반응식

HRID 1754062 반응식
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

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 27545026,7-Dibromobenzo(1,4)dioxanHCID 178418546HCID 178418546, 화합물

생성물 1

HCID 59581200HCID 59581200, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
150 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-d7fc5e04cc1e429bb5396ec9eaa4d9b7
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09169205B2

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