Methanol → 2-(t-Butylamino)-5-chloro-3,6-difluoropyridine

HRID 1274710노트

반응식

HRID 1274710 반응식
CO.Br[C:4]1[C:9]([Cl:10])=[C:8]([F:11])[N:7]=[C:6]([NH:12][C:13]([CH3:16])([CH3:15])[CH3:14])[C:5]=1[F:17]>[Pd].C(N(CC)CC)C>[C:13]([NH:12][C:6]1[C:5]([F:17])=[CH:4][C:9]([Cl:10])=[C:8]([F:11])[N:7]=1)([CH3:16])([CH3:14])[CH3:15]

참가 물질

5

반응물 2

HCID 887MethanolHCID 221211704-Bromo-2-(t-butylamino)-5-chloro-3,6-difluoropyridine

생성물 1

HCID 221211892-(t-Butylamino)-5-chloro-3,6-difluoropyridine수율 98.6%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8471Triethylamine용매

실험 절차

To 30 ml of methanol were added 12.8 g of 4-bromo-2-(t-butylamino)-5-chloro-3,6-difluoropyridine and 2.5 g of triethylamine together with 0.57 g of 10% palladium on carbon, and the mixture was hydrogenated at 50° C. for 5 days. The catalyst was separated by filtration, and the solvent and the like were distilled off under reduced pressure. To the residue was added 80 ml of chloroform, and the mixture was washed with 70 ml of distilled water, and the chloroform layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 9.3 g of the title compound as a brown oil.

후처리

  1. customThe catalyst was separated by filtration
  2. distillationthe solvent and the like were distilled off under reduced pressure
  3. additionTo the residue was added 80 ml of chloroform
  4. washthe mixture was washed with 70 ml of distilled water
  5. dry with materialthe chloroform layer was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-cd5aa83f6ff24021a774203de67e4f55
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06156903

반응 노트

불러오는 중…