Hydrochloric Acid → HCID 12398997、化合物

HRID 2301261ノート

反応式

HRID 2301261 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9](=O)[CH:10](Br)[CH3:11])=[CH:5][CH:4]=1.[CH3:14][O:15][C:16]1[CH:21]=C[C:19](OC)=[CH:18][CH:17]=1.C[N:25](C)C1C=CC=CC=1.Cl>>[CH3:14][O:15][C:16]1[CH:21]=[C:11]2[C:19](=[CH:18][CH:17]=1)[NH:25][C:9]([C:6]1[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=1)=[CH:10]2

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 949N,N-DimethylanilineHCID 90161,4-DimethoxybenzeneHCID 2991022-Bromo-1-(4-methoxyphenyl)propan-1-one

生成物 1

HCID 12398997HCID 12398997、化合物

実験手順

A solution of p-methoxy-2-bromopropiophenone ((1 g, 4.11 mmol) was added to a solution of p-methoxyanisole in N,N dimethylaniline (1.7 g, 13.82 mmol)) and heated under reflux for 3 hours. The reaction mixture was cooled to room temperature, poured into 2N HCl, and extracted with EtOAc. The organic extract was washed with water and dried over Na2SO4. Removal of the solvent under reduced pressure and flash chromatography on SiO2 using CH2Cl2 gave the desired intermediate compound 2.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 3 hours
  3. extractionextracted with EtOAc
  4. extractionThe organic extract
  5. washwas washed with water
  6. dry with materialdried over Na2SO4
  7. customRemoval of the solvent under reduced pressure and flash chromatography on SiO2

出典と根拠

ORDレコード
ord-3def2fc80867488f818c85d12d1174e2
出典データセット
uspto-grants-2002_12
特許番号
US06500669B1

反応ノート

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