Bromine → 3-Bromo-6-(trifluoromethyl)pyridin-2-amine

HRID 451465

반응식

HRID 451465 반응식
[F:1][C:2]([F:11])([F:10])[C:3]1[N:8]=[C:7]([NH2:9])[CH:6]=[CH:5][CH:4]=1.[Br:12]Br>ClCCl>[Br:12][C:6]1[C:7]([NH2:9])=[N:8][C:3]([C:2]([F:1])([F:10])[F:11])=[CH:4][CH:5]=1

참가 물질

4

반응물 2

HCID 24408BromineHCID 8210242-Amino-6-(trifluoromethyl)pyridine

생성물 1

HCID 547588353-Bromo-6-(trifluoromethyl)pyridin-2-amine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 6-(trifluoromethyl)pyridin-2-amine (200 mg, 1.23 mmol) in dichlormethane (2.47 mL) was cooled to 0° C. and bromine (197 mg, 63.4 μL, 1.23 mmol) was slowly added within 30 minutes. After 25 hours at 0° C. the reaction mixture was extracted with saturated Na2S2O3 solution, water and brine, dried over Na2SO4 and concentrated in vacuo. The crude material was purified by flash chromatography over silica gel using CH2Cl2/MeOH (with 10% ammonia) as eluent. The title compound was obtained as a white solid (711 mg, 24%).

후처리

  1. extractionAfter 25 hours at 0° C. the reaction mixture was extracted with saturated Na2S2O3 solution, water and brine
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated in vacuo
  4. customThe crude material was purified by flash chromatography over silica gel

출처 및 근거

ORD 기록
ord-f55ec016212748739785ce7fd3b023d5
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486967B2

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