碳酸钾 → Benzenamine, 4-bromo-2-(4,5-dihydro-3-isoxazolyl)-3-methyl-

HRID 397147

反应方程式

HRID 397147 反应方程式
[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]

参与物

5

反应物 3

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

产物 1

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

试剂、催化剂与溶剂 1

HCID 6342乙腈溶剂

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-48185009ba5b4fda8f47291661fc6cdc
来源数据集
uspto-grants-2003_08
专利号
US06608209B2

关联笔记

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