Potassium Acetate → 6-Bromo-1H-indazole

HRID 1477397

반응식

HRID 1477397 반응식
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

참가 물질

5

반응물 2

HCID 517044Potassium AcetateHCID 805030315-Bromo-2-methylbenzenediazonium tetrafluoroborate

생성물 1

HCID 178424716-Bromo-1H-indazole수율 86.7%

시약·촉매·용매 2

HCID 2855718-Crown-6촉매HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1575ba32906f40b1908a01b86d8971e2
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09403775B2

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