Potassium Carbonate → Benzenamine, 4-bromo-2-(4,5-dihydro-3-isoxazolyl)-3-methyl-

HRID 554684

反応式

HRID 554684 の反応式
[O:1]1[CH2:5][CH2:4][C:3]([C:6]2[C:12]([CH3:13])=[CH:11][CH:10]=[CH:9][C:7]=2[NH2:8])=[N:2]1.C(=O)([O-])[O-].[K+].[K+].[Br-:20].[Br-].[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC>C(#N)C>[Br:20][C:11]1[CH:10]=[CH:9][C:7]([NH2:8])=[C:6]([C:3]2[CH2:4][CH2:5][O:1][N:2]=2)[C:12]=1[CH3:13]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 97940062-(4,5-Dihydroisoxazol-3-yl)-3-methylanilineHCID 23500184Tetra-n-butylammonium tribromide

生成物 1

HCID 9813747Benzenamine, 4-bromo-2-(4,5-dihydro-3-isoxazolyl)-3-methyl-

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

30 g (170 mmol) of 2-(4,5-dihydroisoxazol-3-yl)-3-methylaniline are dissolved in 400 ml of acetonitrile, and 94 g (0.68 mol) of potassium carbonate are added. At temperatures <30° C., 84 g (174 mmol) of tetrabutylammonium tribromide are then added a little at a time, with vigorous stirring. For work-up, the solid is filtered off with suction and the solution is diluted with methylene chloride and extracted with water. The solvent is stripped off and the residue is then taken up again in methyl tert-butyl ether and washed twice with water. The organic phase is dried and concentrated.

後処理

  1. filtrationFor work-up, the solid is filtered off with suction
  2. additionthe solution is diluted with methylene chloride
  3. extractionextracted with water
  4. washwashed twice with water
  5. customThe organic phase is dried
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-bb2e9d6413544412884a23482ff11ebd
出典データセット
uspto-grants-2011_11
特許番号
US08049017B2

関連ノート

読み込み中…