Bromine → 4-Bromo-5-methoxy-2-(trifluoromethyl)pyridine

HRID 1976070노트

반응식

HRID 1976070 반응식
[Br:1]Br.[CH3:3][O:4][C:5]1[CH:6]=[N:7][C:8]([C:15]([F:18])([F:17])[F:16])=[CH:9][C:10]=1[Sn](C)(C)C.[O-]S([O-])=O.[Na+].[Na+]>ClCCl>[Br:1][C:10]1[CH:9]=[C:8]([C:15]([F:18])([F:17])[F:16])[N:7]=[CH:6][C:5]=1[O:4][CH3:3]

참가 물질

5

반응물 3

HCID 24408BromineHCID 24437Sodium SulfiteHCID 22000206HCID 22000206, 화합물

생성물 1

HCID 220001724-Bromo-5-methoxy-2-(trifluoromethyl)pyridine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Bromine (0.52 ml, 10 mmol) was added via syringe to a stirred solution of 3-methoxy-6-trifluoromethyl-4-trimethylstannylpyridine (1.7 g, 5 mmol) in dichloromethane (25 ml). The reaction mixture was stirred for 30 min at room temperature and treated with saturated aqueous Na2SO3 (15 ml). The phases were separated. The aqueous layer was extracted with dichloromethane (2×15 ml). The combined organic extracts were dried (Na2SO4) and concentrated. The residue was purified by chromatography on silica gel (hexane:ethyl acetate 0-15%) to afford 4-bromo-3-methoxy-6-trifluoromethylpyridine as a white solid.

후처리

  1. customThe phases were separated
  2. extractionThe aqueous layer was extracted with dichloromethane (2×15 ml)
  3. dry with materialThe combined organic extracts were dried (Na2SO4)
  4. concentrationconcentrated
  5. customThe residue was purified by chromatography on silica gel (hexane:ethyl acetate 0-15%)

출처 및 근거

ORD 기록
ord-76f1a9e0d81749c380c2edc295b15b35
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06225320B1

반응 노트

불러오는 중…