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

HRID 554684

반응식

HRID 554684 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bb2e9d6413544412884a23482ff11ebd
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08049017B2

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