Stannous Chloride → HCID 20088007, 화합물

HRID 275368노트

반응식

HRID 275368 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:9](=O)[C:10]2[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=2)=[C:6]([CH:8]=1)[NH2:7].[N:18]([O-])=O.[Na+].Cl[Sn]Cl>Cl.O>[Cl:1][C:2]1[CH:8]=[C:6]2[C:5]([C:9]([C:10]3[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=3)=[N:18][NH:7]2)=[CH:4][CH:3]=1

참가 물질

6

반응물 3

HCID 24479Stannous ChlorideHCID 223994925-chloro-2-(4-fluorobenzoyl)anilineHCID 23668193Sodium Nitrite

생성물 1

HCID 20088007HCID 20088007, 화합물수율 50.6%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매2회HCID 962Water용매

실험 절차

To solution of 5-chloro-2-(4-fluorobenzoyl)aniline (5 g) in 6M aqueous HCl (25 ml) was added a solution of NaNO2 (2.5 g) in water (5 ml) at 0°-5° C. under stirring during 15 min. After stirring for further 0.5 h at 0° C. a solution of SnCl2 (20 g) in conc. aqueous HCl (25 ml) was added. The reaction mixture was allowed to heat to room temperature and after 0.5 h the precipitate was filtered off and suspended in 2 N aqueous NaOH. The suspension was filtered and dichloromethane was added to the precipitate. The thus obtained solution was washed with brine and dried (MgSO4). Evaporation of the solvents afforded the title compound (2.5 g) as an oil which was used without further purification. In a corresponding manner the following indazole derivative was prepared: 3-(4-Fluorophenyl)-5-trifluoromethyl-1H-indazole 25b, (oil)

후처리

  1. additionwas added
  2. filtrationwas filtered off
  3. filtrationThe suspension was filtered
  4. additiondichloromethane was added to the precipitate
  5. washThe thus obtained solution was washed with brine
  6. dry with materialdried (MgSO4)
  7. customEvaporation of the solvents

출처 및 근거

ORD 기록
ord-1913f0cdb15f4a8f8f75847c3fae3d06
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05393761

반응 노트

불러오는 중…