Ammonia → 6-Bromopyridine-2-carboxamide

HRID 1717680

반응식

HRID 1717680 반응식
[Br:1][C:2]1[N:7]=[C:6]([C:8]([OH:10])=O)[CH:5]=[CH:4][CH:3]=1.[NH3:11]>S(Cl)(Cl)=O.O1CCOCC1>[Br:1][C:2]1[N:7]=[C:6]([C:8]([NH2:11])=[O:10])[CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 2

HCID 222AmmoniaHCID 5939196-Bromopyridine-2-carboxylic acid

생성물 1

HCID 219614086-Bromopyridine-2-carboxamide수율 45%

시약·촉매·용매 2

HCID 24386Thionyl Chloride용매HCID 312751,4-Dioxane용매

반응 조건

온도
70 °C

실험 절차

6-Bromopicolinic acid (1000 mg, 4.95 mmol) was suspended in thionyl chloride (15 mL) and heated at 70° C. for 5 h. The reaction was cooled to room temperature and the volatiles were condensed under reduced pressure. A solution of ammonia (2M in dioxane (15 mL) was added to the residue and then the solvents were removed under reduced pressure. The crude residue was purified by MPLC with a gradient of 0 to 20% MeOH/dichloromethane to give 6-Bromo-pyridine-2-carboxylic acid amide as a white powder (555 mg, 45%). MS ES (MH+=201.01203.0).

후처리

  1. temperatureThe reaction was cooled to room temperature
  2. customcondensed under reduced pressure
  3. customthe solvents were removed under reduced pressure
  4. customThe crude residue was purified by MPLC with a gradient of 0 to 20% MeOH/dichloromethane

출처 및 근거

ORD 기록
ord-ef965202b9f4400aa9f46cf1ee70eb7f
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07803956B2

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