乙酸钾 → 6-溴吲唑

HRID 473782

反应方程式

HRID 473782 反应方程式
F[B-](F)(F)F.[Br:6][C:7]1[CH:8]=[CH:9][C:10]([CH3:15])=[C:11]([N+:13]#[N:14])[CH:12]=1.C([O-])(=O)C.[K+]>C(Cl)(Cl)Cl.C1OCCOCCOCCOCCOCCOC1>[Br:6][C:7]1[CH:12]=[C:11]2[C:10]([CH:15]=[N:14][NH:13]2)=[CH:9][CH:8]=1

参与物

5

反应物 2

HCID 517044乙酸钾HCID 805030315-Bromo-2-methylbenzenediazonium tetrafluoroborate

产物 1

HCID 178424716-溴吲唑收率 86.7%

试剂、催化剂与溶剂 2

HCID 2855718-冠醚-6催化剂HCID 6212三氯甲烷溶剂

实验过程

5-Bromo-2-methylphenyldiazonium tetrafluoroborate (1.50 g) was added to a mixture of potassium acetate (1.0 g) and 18-crown-6 (70 mg) in chloroform (50 mL) at room temperature in portions and then the reaction was stirred for 2 h. The resulting mixture was filtered and washed with chloroform. The filtrate was concentrated, and the residue was dissolved in diethyl ether, which was then washed with water, brine, dried, and the solvent was removed to give the product 6-bromoindazole (0.9 g). The product was used in the next step without further purification.

后处理

  1. filtrationThe resulting mixture was filtered
  2. washwashed with chloroform
  3. concentrationThe filtrate was concentrated
  4. dissolutionthe residue was dissolved in diethyl ether
  5. washwhich was then washed with water, brine
  6. customdried
  7. customthe solvent was removed

来源与证据

ORD记录
ord-66804a95cd6e4a919da44c3a3ec0d8a7
来源数据集
uspto-grants-2014_01
专利号
US08637497B2

关联笔记

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